ANNUAL REPORT FY 86 ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY OFFICE OF RESEARCH AND DEVELOPMENT U.S. ENVIRONMENTAL PROTECTION AGENCY CINCINNATI, OHIO 45268 ------- ^e0SBv © \ ^\|/^ 1 UNITED STATES ENVIRONMENTAL PROTECTION AGENCY OFFICE OF RESEARCH AND DEVELOPMENT ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY CINCINNATI. OHIO 45268 S} z/eodon!* DATE: December 15, 1986 SUBJECT: FY86 Environmental Monitoring and Support Laboratory - Cincinnati (EMSL-Cincinnati) Annual Report FROM: Robert L. Booth, Director /. Environmental Monitoring and Support / Laboratory - Cincinnati TO: SEE BELOW Merry Christmas and Happy New Year to all of you! The following pages summarize the purpose of our projects, approach used, and accomplishments. If additional copies are needed for distribution to other key staff members, please call us at 684-7301. Selected highlights from FY86 are: ° Published and distributed "Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms" (EPA- 600/4-85-014). 0 Revised Chapter 8 and Chapter 9 of the "USEPA Manual of Methods for Virology" The latter chapter has been divided into two new chapters, the first of which was completed and has received Agency clearance, "Cell Culture Preparation and Maintenance". The second part, "Cell Culture Procedures for Virus Assay" is near completion and distribution will be made in FY87. ° Established a computer-based information exchange system (bulletin board) to provide access by the user community to IBM PC-AT compatible versions of a biological statistics package currently containing 45 programs. o Prepared draft interim report on "Evaluation of a Microbial Test for Muta- genicity of Wastewater" which describes preliminary precision and accuracy determinations performed with the Ames test. 0 Forwarded the final report on the comparison of the hydrophobic grid membrane filter (HGMF) with the standard membrane filter and submitted for journal publication. ° Completed laboratory Performance Evaluation (PE) Studies Water Pollution (WP) 015 and 016 and distributed reports to the participants on how they performed on the unknown samples. ------- 2 0 Completed Water Supply (WS) 18 and WS19 PE studies for certification under the requirements of the Safe Drinking Water Act (SDWA). Overall, 2000 laboratories participated in these studies for measuring the contaminants near the maximum contaminant level (MCL). 0 Completed WSM07 and WSM08 microbiological PE studies. Approximately 100 regional and state laboratories participated in these studies for total coliforms at two concentration levels. 0 Provided over 285,000 WP quality control (QC) samples to U. S. Environmental Protection Agency (USEPA), regional, state, and USEPA contractors. Addition- ally, distributed approximately 75,000 spiking/calibration solutions in support of regulations under the Clean Water Act and Consent Decree for Priority Pollutants. 0 Provided final report to each participating laboratory in the Discharge Monitoring Report-Quality Assurance (DMR-QA) study 6 (approximately 7400 major National Pollutant Discharge Elimination System (NPDES) dischargers). 0 Prepared and distributed three special interlaboratory comparison studies to evaluate Resource Conservation and Recovery Act (RCRA) contract laboratories. 0 Prepared and distributed special inorganic and organic PE samples for con- tract laboratories involved in groundwater monitoring. 0 Provided full-volume natural wastewater samples spiked with organic toxi- cants to Superfund contract laboratories on a quarterly basis as a measure of their potential performance. 0 Completed a special project to develop a method for acid soluble metals and presented an overview at the Society for Applied Spectroscopy Seminar on Atomic Spectroscopy. ° Provided a "Report on Evaluation of Metals Dissolution for Chromium" to the Office of Solid Waste (0SW). 0 Redrafted and forwarded final rule of the October 26, 1984, Interim rule on priority pollutants to the Office of General Counsel and the Work Group for comment. Maintained a continuing project to correct inadequacies of 304(h) methods for application to specific matrices. ° Submitted a paper for publication entitled "A Universal Kriging Program for the IBM-PC for Use in Monitoring Sediments 1n Lakes", as part of the Symposium Proceedi ngs. ° Processed a total of 74 requests for alternate test procedures (ATPs), 51 of which were related to NPDES and 23 to the SDWA requirements. Of the total, 34 were approved; 6, disapproved; 24 required additional data; 4, pending; and 6 were not-germane (not ATPs). ------- 3 ° Transmitted a revised manual entitled "Methods for Volatile Organic Chemicals" to the Office of Drinking Water. ° Held two certification training courses for state and regional persons: Drinking Water Chemical Laboratory Certification Course and Drinking Water Microbiological Laboratory Certification Course. ° Made on-site visits to four regional laboratories during the fiscal year. At the request of Regions 2 and 8, also evaluated the United States Geological Survey laboratory in Denver, Colorado, for compliance with drinking water regulations. ° Continued the evaluation and testing of several SW-846 methods. ° Participated in the National Inorganic and Radiological Survey by providing analytical results for 37 elements on 475 samples totalling 22,191 analyses, and analyzed 1176 radionuclide samples. ° Developed an enzyme linked immunosorbent assay technique for the measurement of dioxins and furans. Plans are to field test this immunochemical method in FY87. ° Provided methods manual report on "Standard Methods for Collection and Analysis of Precipitation". Attachments (66): Annual Report for Each Project ADDRESSEES: Vaun Newill, Assistant Administrator, Office of Research and Development (RD-672) Donald Ehreth, Deputy Assistant Administrator, Office of Research and Develop- ment (RD-672) Courtney Riordan, Director, Office of Acid Deposition, Environmental Monitor- ing, and Quality Assurance (RD-680) H. Matthew Bills, Deputy Director, Office of Acid Deposition, Environmental Monitoring, and Quality Assurance (RD-680) Alan Neuschatz, Special Assistant to the Director, Office of Acid Deposition, Environmental Monitoring, and Quality Assurance (RD-680) Paul Palm, Chief, Program Operations Staff, Office of Acid Deposition, Environ- mental Monitoring, and Quality Assurance (RD-680) Stanley Blacker, Director, Quality Assurance Management Staff, Office of Acid Deposition, Environmental Monitoring, and Quality Assurance (RD-680) Gary Foley, Director, Acid Deposition and Atmospheric Research Division, Office of Acid Deposition, Environmental Monitoring, and Quality Assurance (RD-680) Charles Brunot, Director, Environmental Monitoring Systems Division, Office of Acid Deposition, Environmental Monitoring, and Quality Assurance (RD-680) ------- 4 Richard Nalesnik, Special Assistant to the Director, Environmental Monitoring Systems Division, Office of Acid Deposition, Environmental Monitoring, and Quality Assurance (RD-680) Charles Plost, Chemist, Environmental Monitoring Systems Division, Office of Acid Deposition, Environmental Monitoring, and Quality Assurance (RD-680) Vernon Laurie, Program Analyst, Environmental Monitoring Systems Division, Office of Acid Deposition, Environmental Monitoring, and Quality Assurance (RD-680) John Koutsandreas, Environmental Scientist, Environmental Monitoring Systems Division, Office of Acid Deposition, Environmental Monitoring, and Quality Assurance (RD-680) Michael Dellarco, Environmental Scientist, Environmental Monitoring Systems Division, Office of Acid Deposition, Environmental Monitoring, and Quality Assurance (RD-680) David Graham, Environmental Monitoring Systems Division, Office of Acid Deposi- tion, Environmental Monitoring, and Quality Assurance (RD-680) Jack Puzak, Acting Director, Environmental Monitoring Systems Laboratory - Research Triangle Park Erich Bretthauer, Director, Environmental Monitoring Systems Laboratory - Las Vegas Alfred Ellison, Director, Atmospheric Sciences Research Laboratory - Research Triangle Park Thomas Hauser, Director, Hazardous Waste Engineering Research Laboratory - Cincinnati Francis Mayo, Director, Water Engineering Research Laboratory - Cincinnati Lowell Van Den Berg, Director, Technical Support Division, Office of Drinking Water Herbert Brass, Chief, Drinking Water Quality Assessment Branch, Technical Sup- port Division, Office of Drinking Water Calvin Lawrence, Director, Center for Environmental Research Information Frank Princiotta, Director, Air and Energy Engineering Research Laboratory - Research Triangle Park Lester Grant, Director, Environmental Criteria and Assessment Office - Research Triangle Park Jerry Stara, Director, Environmental Criteria and Assessment Office - Cincinnati Rosemarie Russo, Director, Environmental Research Laboratory - Athens Clinton Hall, Director, Robert S. Kerr Environmental Research Laboratory - Ada Thomas Murphy, Director, Environmental Research Laboratory - Corvallis Norbert Jaworski, Director, Environmental Research Laboratory - Narragansett Gilman Velth, Acting Director, Environmental Research Laboratory - Duluth Henry Enos, Director, Environmental Research Laboratory - Gulf Breeze F. Gordon Hueter, Director, Health Effects Research Laboratory - Research Triangle Park Rebecca Hanmer, Deputy Assistant Administrator for Water (WH-556) Joseph Cotruvo, Director, Criteria and Standards Division, Office of Drinking Water (WH-550) Arthur Perler, Chief, Science and Technology Branch, Criteria and Standards Division, Office of Drinking Water (WH-550) ------- 5 Irwin Pomerantz, Quality Assurance Officer, Science and Technology Branch, Criteria and Standards Division, Office of Drinking Water (WH-550) Maria Gomez-Taylor, Chemist. Health Effects Branch, Criteria and Standards Division, Office of Drinking Water (WH-550) Paul Berger, Microbiologist, Health Effects Branch, Criteria and Standards Division, Office of Drinking Water (WH-550) Arnold Kuzmack, Director, Program Development and Evaluation Division, Office of Drinking Water (WH-550) Marian Ml ay, Director, Office of Ground-Water Protection (WH-550G) Tudor Davies, Director, Office of Marine and Estuarine Protection (WH-556M) Michael Quigley, Director, Office of Municipal Pollution Control (WH-546) James Elder, Director, Office of Water Enforcement and Permits (EN-335) J. William Jordan, Director, Enforcement Division, Office of Water Enforcement and Permits (EN-338) Martha Prothro, Director, Permits Division, Office of Water Enforcement and Permits (EN-336) William Brandes, Permits Division, Office of Water Enforcement and Permits (EN-336) Geoffrey Grubs, Permits Division, Office of Water Enforcement and Permits (EN-336) Marcia Williams, Director, Office of Solid Waste (WH-562) Jeffery Denit, Deputy Director, Office of Solid Waste (WH-562) David Friedman, Manager, Methods Program, Characterization and Assessment Division, Office of Solid Waste (WH-562B) Paul Friedman, Characterization and Assessment Division, Office of Solid Waste (WH-562B) Florence Richardson, Quality Assurance Officer, Characterization and Assessment Division, Office of Solid Waste (WH-562B) Stanley Kovell, Chief, Analytical Support Branch, Hazardous Response Support Division, Office of Program Management (WH-548A) William Garetz, Environmental Results Branch, Management Systems Division, Office of Management Systems and Evaluation (PM-222A) R. Augustus Edwards, Deputy Assistant Administrator, Office of External Affairs (A-100EA) Hugh McKinnon, Co-Chairperson, Consolidated Water Research Committee (RD-682) Curtis Harlin, Office of Regulatory Support (RD-672) Victoria Price, Office of Water (WH-556) William Whittington, Director, Office of Water Regulations and Standards (WH-551) Devereaux Barnes, Director, Industrial Technology Division, Office of Water Regulations and Standards (WH-552) Frederic Leutner, Acting Director, Monitoring and Data Support Division, Office of Water Regulations and Standards (WH-553) Timothy Stuart, Chief, Monitoring Branch, Monitoring and Data Support Division, Office of Water Regulations and Standards (WH-553) Edmund Notzon, Director, Criteria and Standards Division, Office of Water Regulations and Standards (WH-585) James McDermott, Scientific and Technical Advisor, Criteria and Standards Division, Office of Water Regulations and Standards (WH-585) ------- 6 David Davis, Deputy Director, Office of Federal Activities (A-104) Robert Wolcott, Director, Regulatory and Economic Analysis Division, Office of Policy Analysis, Office of Policy, Planning, and Evaluation (PM-221) Samuel Bryant, Program Analyst, Budget Division, Office of the Comptroller (PM-225) Richard Frank, Program Analyst, Planning Staff, Office of Research Program Management (RD-674) Brenda Washington, Management Analyst, Program Coordination Staff, Office of Research Program Management (RD-674) Michael Deland, Regional Administrator, U. S. Environmental Protection Agency, Region 1, Attention: Lester Sutton, Research and Development Contact Paul Keough, Deputy Regional Administrator, U. S. Environmental Protection Agency, Region 1 Christopher Dagget, Regional Administrator, U. S. Environmental Protection Agency, Region 2, Attention: Barbara Metzger, Research and Development Contact William Muszynski, Deputy Regional Administrator, U. S. Environmental Protection Agency, Region 2 James Seif, Regional Administrator, U. S. Environmental Protection Agency, Region 3, Attention: John Ruggero, Research and Development Contact Stanley Laskowski, Deputy Regional Administrator, U. S. Environmental Protec- tion Agency, Region 3 Jack Ravan, Regional Administrator, U. S. Environmental Protection Agency, Region 4, Attention: David Hopkins, Research and Development Contact Lee DeHihns, Deputy Regional Administrator, U. S. Environmental Protection Agency, Region 4 Valdas Adamkus, Regional Administrator, U. S. Environmental Protection Agency, Region 5, Attention: William Sanders, III, Research and Development Contact Frances Phillips, Acting Regional Administrator, U. S. Environmental Protection Agency, Region 6, Attention: Oscar Ramirez, Jr., Research and Development Contact Morris Kay, Regional Administrator, U. S. Environmental Protection Agency, Region 7, Attention: Ralph Hazel, Research and Development Contact William R1ce, Deputy Regional Administrator, U. S. Environmental Protection Agency, Region 7 John Welles, Regional Administrator, U. S. Environmental Protection Agency, Region 8, Attention: Denis Nelson, Research and Development Contact Alexandra Smith, Deputy Regional Administrator, U. S. Environmental Protection Agency, Region 8 Judith Ayres, Regional Administrator, U. S. Environmental Protection Agency, Region 9, Attention: Arnold Den, Research and Development Contact John Wise, Deputy Regional Administrator, U. S. Environmental Protection Agency, Region 9 Robbie Russell, Regional Administrator, U. S. Environmental Protection Agency, Region 10, Attention: Carolyn Wilson, Research and Development Contact Ralph Bauer, Deputy Regional Administrator, U. S. Environmental Protection Agency, Region 10 Edward Conley, Director, Environmental Services Division, U. S. Environmental Protection Agency, Region 1 ------- 7 Barbara Metzger, Director, Environmental Services Division, U. S. Environmental Protection Agency, Region 2 Greene Jones, Director, Environmental Services Division, U. S. Environmental Protection Agency, Region 3 James Finger, Director, Environmental Services Division, U. S. Environmental Protection Agency, Region 4 William Sanders, III, Director, Environmental Services Division, U. S. Envi- ronmental Protection Agency, Region 5 Russell Rhoades, Director, Environmental Services Division, U. S. Environmental Protection Agency, Region 6 John Wicklund, Director, Environmental Services Division, U. S. Environmental Protection Agency, Region 7 James Lehr, Director, Environmental Services Division, U. S. Environmental Protection Agency, Region 8 David Mowday, Deputy Director, Office of Policy and Management, U. S. Environ- mental Protection Agency, Region 9 William Schmidt, Acting Director, Environmental Services Division, U. S. Envi- ronmental Protection Agency, Region 10 Michael Mastracci, Director, Regional Services Staff, Office of Research Program Management (RD-675) Robert Booth, Director, Environmental Monitoring and Support Laboratory - Cincinnati Thomas Clark, Deputy Director, Environmental Monitoring and Support Laboratory - Cincinnati Terry Grady, Chemist, Equivalency Staff, Environmental Monitoring and Support Laboratory - Cincinnati Robert Graves, Technical Advisor, Environmental Monitoring and Support Laboratory - Cincinnati Daniel Bender, Quality Assurance Management Staff Liaison, Environmental Monitoring and Support Laboratory - Cincinnati Teresa Firestone, Budget Analyst, Environmental Monitoring and Support Laboratory - Cincinnati James Llchtenberg, Chief, Physical and Chemical Methods Branch James Longbottom, Chief, Organic Analyses Section, Physical and Chemical Methods Branch Gerald McKee, Chief, Inorganic Analyses Section, Physical and Chemical Methods Branch William Budde, Chief, Advanced Instrumentation Section, Physical and Chemical Methods Branch Joseph Roesler, Environmental Engineer, Sampling and Field Measurements Section, Physical and Chemical Methods Branch John Winter, Chief, Quality Assurance Branch Edward Berg, Chief, Project Management Section, Quality Assurance Branch Harold Clements, Chief, Evaluation Section, Quality Assurance Branch Cornelius Weber, Chief, Biological Methods Branch Robert Safferman, Chief, Virology Section, Biological Methods Branch Robert Bordner, Chief, Microbiology Section, Biological Methods Branch William Horning, Chief, Aquatic Biology Section, Biological Methods Branch ------- FY-86 OUTPUT PLAN AQUATIC BIOLOGY SECTION, BMB, EMSL-CINCINNATI WATER QUALITY-MONITORING SYSTEMS AND QUALITY ASSURANCE, BIO Page J of 76 PE# OUTPUT Reference Biological Methods - Water Quality ORD Contact Name W.B. Horning rTc 778-8-350 FIS No. Resources: $(000) 417 K PFT OPFT PFTE6.9 OPFTE Project 01 ANNUAL REPORT - FY86 The manual, "Short-Term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms," (EPA-600/4-85-014) was published and distributed. A manuscript, "Toxicity Reduction by Municipal Wastewater Treatment in Ohio," was completed for submission to the Journal of the Water Pollution Control Federation. This report was the result of a cooperative study between EMSL-Cincinnati, the Water Engineering Research Laboratory - Cincinnati, and the Ohio Environmental Protection Agency. The reduction of toxicity by municipal waste treatment plants was determined by measuring influent and effluent toxicity. A computer-based information exchange system (bulletin board) was established to provide access by the user community to IBM PC-AT compatible versions of a biological statistics package (BSP) at the EMSL-Cincinnati Newtown Facility, which currently contains 45 programs. Approximately 80 requests have been received for the BSP, and 57 individuals have downloaded the BSP directly from the IBM PC. The Aquatic Biology Section participated in a 10-laboratory study of the precision of the seven-day fathead minnow larval survival and growth test sponsored by the American Petroleum Institute and the Electric Power Research Institute in cooperation with the USEPA and the Chemical Manufacturers Association. The study was coordinated by thev Battelle-Columbus Laboratories, and involved testing of seven reference materials, including effluents, over an eight-month period. The EMSL-Cincinnati Newtown Facility provided test animals for five of the participating laboratories. The annual review of the literature on "Effects of Pollution on Freshwater Organisms," was completed for publication in the Journal of the Water Pollution Control Federation, as part of a joint effort with the Environmental Research Laboratory - Duluth. ------- Page 2 of Project No. 01 Page 2 of 76 A report, "Taxonomy of Ceriodaphnia (Crustacea: Cladocera) in U.S. Environmental Protection Agency Cultures," was completed. The manuscript, "Short-term Fish and Amphibian Embryo-larval Tests for Determining the Effects of Toxicant Stress on Early Life Stages and Estimating Chronic Values for Single Compounds and Complex Effluents," based on research funded by EMSL-Cincinnati under a cooperative agreement with the University of Kentucky, Lexington, was published by Dr. Wesley Birge and associates in the journal, Environmental Toxicology and Chemistry. Funding for a new cooperative agreement with the University of Kentucky, Lexington, entitled "Improvements in Methods for Toxicological Monitoring of NPDES Effluents with Emphasis on Short-Term Chronic Procedures," was also approved. A formal paper, "A Short-term Chronic Toxicity Test Using Daphnia magna," was presented at the Tenth ASTM Aquatic Toxicity and Hazard Assessment Symposium. A poster session, "Comparative Evaluation of Two Short-term Fathead Minnow Tests for Measuring Chronic Toxicity to Three Reference Toxicants," was also presented. Both will be submitted to peer-reviewed publications. Cultures for four marine species have been established using "Forty Fathoms" artificial sea salts. These species are: Mysid shrimp (Mysidopsis bahia), sea urchin (Arbacia punctulata), sheepshead minnow (Cyprinodon variegatus) and the red macro-alga Champia parvula. Short-term chronic toxicity tests with these species are being evaluated. The Aquatic Biology Section supplied 192,000 fathead minnows (in various life stages) to other USEPA and state laboratories, universities, USEPA grantees or contractors, and other Federal agencies performing toxicity tests with effluents or pure compounds in USEPA-related activities. A meeting of the EMSL-Cincinnati-sponsored Agency Biological Advisory Committee was held in Cincinnati. The meeting was attended by biologists from the regional programs, research laboratories, and headquarters program offices. Aquatic Biologists participated in on-site visits to the Environmental Services Division, Region 3, Wheeling Office, and Regions 5 and 6, to determine compliance with methodology and quality assurance practices for NPDES and other biomonitoring activities. ------- FY-86 OUTPUT PLAN MICROBIOLOGY SECTION, BMB, EMSL-CINCINNATI WATER QUALITY - MONITORING SYSTEMS AND QUALITY ASSURANCE Page __3 of 76 PIt B101 ORO Contact OUTPl/T Reference Biological Methods - Water Quality Name R. Bordner FTS Ho. 68fl-J31 Resources: 5(000) 265.6Kppj 4.8 QPFT 0.0 PFTE 4.8 OPFTE 0.0 Project 02 ANNUAL REPORT - FY 86 The final report on the comparison of the hydrophobic-grid membrane filter (HGMF) with the standard membrane filter (MF) and most probable number (MPN) procedures was forwarded to the Office of Water and submitted to Applied and Environmental Microbiology for publication. The standard MF and HGMF procedures did not produce significantly different results. A draft interim report on "Evaluation of a Microbial Test for Mutagenicity of Wastewater" was prepared. The report describes preliminary precision and accuracy determinations performed with the Ames test, and confirms the inhousc capability to run this test. The test will be used as a reference method for evaluation of other proposed short-term tests for microbial mutagenicity. Successful practice trials using resin-packed glass and stainless steel columns were completed as the initial step in the task to compare the efficiency of mutagen recovery by three methods of sample preparation used in performing the Ames Test. A draft of the interim report entitled "Precision and Relative Accuracy of th( Membrane Filter and Most Probable Number Total Coliform Methods with Several Water Types" was completed and awaits typing of several tables. The positive tube MPN data from this project were tabulated and given to the Computer Services and Systems Division to calculate the MPN values using the upgraded computer program developed for EMSL-Cincinnati under the statistical services contract. A separate report will be prepared describing the application and availability of the computer program for calculating MPN results. The project plan and quality assurance plan for the project entitled "Evaluation of Improved MF methods for Fecal Coliforms in Chlorinated Effluents" were prepared, and cultures of Escherichia coli and several other fecal positive organisms were isolated and characterized for use in evaluating the fecal coliform media. ------- Page 2 of Project No. 02 Page 4 of 76 The task to develop, evaluate, and standardize methods for the detection and enumeration of salmonellae in sludges, wastewater, and leachates was initiated with an on-line literature search of several data bases. A feasibility study was conducted to determine if the HGMF could be used in a quantitative technique for salmonellae. The procedure shows promise based on preliminary results from a raw primary sludge sample. In collaboration with the Quality Assurance Branch, EMSL-Cincinnati, and the Toxicology and Microbiology Division, Health Effects Research Laboratory - Research Triangle Park, descriptions of two agency test methods for recreational waters, "Test Methods for Escherichia coli and Enterococci in Water by the Membrane Filter Procedure" were prepared for publication, and round-robin testing was conducted to determine the precision, bias, specificity, and upper counting range of the methods. Two abstracts were prepared and submitted to the American Society for Microbiology for presentation at the Annual Meeting in Atlanta, Georgia, March 1987. The abstracts describe research on development of a new screening test to determine the acceptability of 0.45 um MFs for water analyses, and a comparison of three selective media for isolation and enumeration of Staphylococcus aureus in swimming pool waters. In line with EMSL-Cincinnati1s lead role in analytical quality assurance for the Agency, quality control checks were run on several lots of MFs. Problems with colony spreading, non-wetting, ink grid toxicity, and other unacceptable effects were observed. Procedures were initiated to study these deficiencies with the electron microscope. A comparison of commercially-available, disposable dilution bottles containing phosphate buffer (PB) and 0.1 percent peptone buffer with inhouse prepared dilution blanks containing the same two buffers was conducted in response to a request for approval through the Equivalency Program. The contents of>both commercially-available buffers were sterile. Inhouse and commercially prepared PB dilution blanks recovered Escherichia aerogenes equally well and a comparison of peptone waters showed similar results. However, commercially-prepared peptone blanks contained less peptone than specified. ------- FY-86 OUTPUT PLAN VIROLOGY SECTION, BMB, EMSL-CI NCINNATI WATER QUALITY-MONITORING SYSTEMS AND QUALITY ASSURANCE, B101 Page 5 of 76_ PE# OUTPUT Reference Biological Methods - Water Quality ORD Contact ^tineR.S. Safferma FTS No. 684-7337 Resources: $(000) 332,6 K PFT 4-° OPFT T-8 PFTE 4-0 OPFTE^-8 Project 03 ANNUAL REPORT FY86 The report, "Optimization of the BGM Cell Line Culture and Viral Assay Procedure for Monitoring Viruses in the Environment", was published in the April issue of "Applied and Environmental Microbiology". Presented in this report are standardized procedures for cultivating the Buffalo green monkey (BGM) kidney cell line and for its use in assaying waterborne viruses. Also reported were the superiority of the cell line for virus isolations when compared to nine other cell types and the finding that certain media and additives tended to increase BGM cell sensitivity to a specific group of viruses. The report, "Recovery of Viruses from Water by a Modified Flocculation Procedure for Second-Step Concentration", was published in the June issue of "Applied and Environmental Microbiology." The study was undertaken because a change in the commercial processing of beef extract had resulted in a reduction in virus recovery efficiencies. Investigation of the problem led to the finding that the addition of Celite analytical filter-aid corrected this deficiency. The operational capacity of a fluid proportioner currently used in virus concentration systems was compared with that of a recently developed in-line injector system. The in-line injector system proved to be much less cumbersome and much more economical. The revised Chapter 8 of the "USEPA Manual of Methods for Virology" was prepared for distribution. This new chapter provides improved methodology that can be applied to the recovery of viruses from samples of sewage, effluents and waters found toxic to mammalian cells used for the assay of enteroviruses, and can also be used to remove deeply colored samples which, if left on the cell monolayers, would result in inaccurate plaque counts. Chapter 9 of the manual is now in the process of being revised. The original chapter has been divided into two chapters, and the first of these chapters, "Cell Culture Preparation and Maintenance", was completed and has received Agency clearance. ------- Page Z of Project No. 03 Page 6 of 76 Round-robin tests involving nine laboratories were completed with methodology for detecting viruses in soil, under the jurisdiction of the Task Group on Viruses in Solids, American Society for Testing and Materials. An internal report, "Method for Mammalian Cell Toxicity Test", was prepared which describes a technique to determine the threshold cytotoxicity of water and wastewater . Draft reports on the optimization of the suspended cell technique for virus enumeration, and for recovery of viruses from sewage sludges, were prepared and are in internal review and revision. Virus analyses were performed for the Water Engineering Research Laboratory - Cincinnati (WERL-Cincinnati) using outputs from a feed-and-draw sludge operation at the USEPA's Test and Evaluation Facility in Cincinnati. Samples were also analyzed for WERL-Cincinnati to determine whether retrofitted anaerobic and aerobic wastewater sludge digesters would meet the pathogenic bacteria and enteric virus reduction requirement of USEPA Criteria 40 CFR, Part 257, Appendix 11(A). Results thus far indicated good reproducibi1ity of data sets and a pronounced difference in the virus removal efficiency between the conventional and modified systems. Technical support was provided to the South Carolina Department of Health and Environment Control concerning enteric virus monitoring of secondary sewage effluents at Hilton Head. Nine water samples collected from the New York Bight by Region 2 were analyzed for viruses. A guest worker in the Virology Section was awarded a Master of Science degree from the University of Cincinnati. Her thesis, entitled "The Evaluation of Reconcentration Methods in Monitoring for Human Enteric Viruses in Environmental Samples," was based on research conducted in our laboratory under the guidance of the Virology Section staff. ------- APPROACH Water Quality - DU B107 Page 7 of j$_ PE# AAPB1A Complete semi-annual OUTPUT and report on USEPA, A. performance evaluation studies state and local laboratories. C. ORD Contact Name Harold Clements FTS No. 684-7325 Resources B. $(000) 50 PFT 0.8 OPFT 0.2 PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 04 Inhouse Task: Develop Performance Evaluation (PE) Samples. Purpose: Provide a system for evaluating the skills of USEPA, USEPA contractor, state, and local laboratories analyzing samples as required under the Clean Water Act. Approach: As part of the Mandatory Quality Assurance (QA) Program, PE samples are designed, developed, produced, and verified by repeated analyses. These stable, homogeneous sample concentrates with known true values are then used in formal studies to evaluate 500-900 USEPA, state, and local laboratories, based on on requests from regional QA coordinators, states, and USEPA project officers. Accomplishments: New PE ampuls were prepared for total phenolics (3,000 ampuls), total residual chlorine (6,000 ampuls) and minerals (24,000 ampuls). Analyses of the above samples verified that the theoretical concentrations and the analyzed values agree. Final verification analyses were completed for all samples before distribution in Water Pollution (WP) Studies 16 and 17. Samples were sent to 546 laboratories in WP Study 16 and 830 laboratories in WP Study 17. Most of these laboratories participated in the organic and the inorganic portion of the tests which comprised 73 parameters/ analytes at two separate concentrations. Status: Annual Report on Design, Development, and Distribution of PE Samples Completed (12/85) ------- Page 2 of Project No. 04 ~ Page 8 of 76 APPROACH PE# MFB1A Water Quality - DU B107 Complete semi-annual performance evaluation studies C. ORD Contact OUTPUT and report on EPA, state and local laboratories. Name Paul Britton A . FTS No. 684-7325 RpQrturrp^ B. $(000) 255 PFT 4.1 OPFT 0 PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 04 Task: Conduct Water Pollution (WP) Laboratory Performance Evaluation Studies. Purpose: To provide an objective measure of the ability of the USEPA, USEPA contractor, state, and local laboratories that generate water quality data to demonstrate acceptable performance. Approach: Samples are designed, prepared, and distributed in interlaboratory studies offered twice each year to USEPA, state, USEPA contract laboratories, and additional laboratories elected by the USEPA Regions. These studies cover a broad group of ambient monitoring analytes including: 21 trace metals, 12 minerals, 5 nutrients, 3 demands, 2 polychlorinated biphenyls (PCBs), 8 pesticides, 11 volatile organics, 6 aromatic purgeables, total cyanide, non- filterable residue, oil and grease, total phenolics, and total residual chlorine. Analytical results are compared with acceptance and warning limits based upon the known true concentrations and results from the current and past studies. Performance in these studies is used to identify problems so they can be investigated and resolved. Accomplishments: During the year, reports were generated for studies WP015 and WP016, with 525 and 381 participating laboratories, respectively. Study WP017 was initiated and will be completed next year. There were 73 parameters offered for analyses, most at two separate concentrations in each study. Status: Individual Laboratory Performance Evaluation Completed Reports Distributed to Participants in Study (7/86) WP015 and Study WP016 ------- Page 3 of Project No. 04 APPROACH Water Quality - DU B107 Page 9 of 76 PE# TOFB1A OUTPUT QA Sample Repository A. C. ORD Contact Name Harry Kolde FTS No. 684-7325 Resources B. R/D $30K $(000) 39.7 PFT 0.2 OPFT PFTE OPFTE Extramural Task; Purpose: Approach: Accomplishments: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 04 USEPA Repository for Toxic and Hazardous Materials, Produce and Distribute Calibration Standards and Surrogates. The USEPA Repository for Toxic and Hazardous Materials provides spiking/calibration solutions of organic compounds in support of regulations under the Clean Water Act and Consent Decree for Priority Pollutants. Compounds of interest to the 304(h) and priority pollutant regulations are purchased or synthesized, then purified, dissolved in the appropriate solvent and dispensed in 5 mL ampuls. The verity of pure compounds and concentrations of the compounds in the ampuls are verified by referee laboratories. Upon verification, spiking/ calibration solutions are distributed to USEPA, USEPA contractor, state, and local laboratories monitoring the environment. 1. Spiking/calibration solutions for 110 of 111 organic priority pollutants under the Consent Decree are available for use by USEPA, USEPA contractor, regional, state, and local laboratories. The remaining one is now being analyzed by referee laboratories. 2. In FY86 75,200 spiking/calibration solutions were distributed to 1553 USEPA, regional, state, and local laboratories engaged in environmental monitoring. Compounds available for distribution are listed in USEPA Quality Assurance Newsletter. 3. Of the 16 gas chromatograph/mass spectrometer (GC/MS) surrogates specified in USEPA Methods 624 and 625, all are now available for use as calibration standards. 4. Native and 13c-iabeled 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) are available as calibration standards. Status: Annual Report on the Repository Completed (12/85) ------- Page 4 of Project No. 4 APPROACH Water Quality - DU B107 Page 10 of 76 PE# TOFB1A OUTPUT QC Sample Program A. C. ORD Contact Name Ray Wesselman FTS No. 684-7325 Resources B. R/D $20K $(000) 29.7 PFT 0.2 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 04 Extramural Task: Develop, Analyze, and Distribute Quality Control (QC) Samples for Water-related Analytes. QC samples are provided to USEPA, USEPA contractors, regional, state, and local laboratories as a check on the technique and analytical methodology. Such checks are necessary to measure quality of data being generated in carrying out mandates of the Clean Water Act and Consent Decree for Priority Pollutants. Bionetics, Inc., the technical service contractor, develops, produces, and distributes QC samples. Development of new sample types requires chemicals of the highest purity which are obtained from best sources including the USEPA Repository for Toxic and Hazardous Materials. The methodology for the compounds of interest are selected, retention time studies are conducted, and finally combining groups of organic compounds to minimize overlapping gas chromatography (GC) peaks. Zero, 45-, and 90-day stability studies are conducted. Those compounds proven stable are produced at one concentration level in lots of 5,000. Random samples are withdrawn during production and sent to referee laboratories for verification analyses. Upon verification, the new sample series is listed in the USEPA Quality Assurance (QA) Newsletter and distributed to requesters. Accomplishments: A total of 285,167 water pollution QC samples were distributed for all programs containing such analytes as trace metals for atomic absorption (AA) and inductively-coupled plasma (ICP) analyses, demands, nutrients, suspended solids, minerals, 109 priority pollutants for USEPA 600 series methodology, GC/mass spectrometer (MS) base neutrals, acids and purgeables, natural matrix samples such as polychlorinated biphenyls (PCBs) in oil and fish, metals and pesticides in fish, phenols, cyanide, and crude oils. Samples listed in the USEPA QA Newsletter are distributed to USEPA, USEPA contractor, state, and local laboratories. A total of 181,000 ampuls were produced to replenish depleted inventories and included such QC series as trace metals, cyanide, PCBs in oil and acetone, pesticides, demand, nutrients, and seven volatile organic series. Purpose: Approach: ------- Page 5 of Project No. 04 APPROACH Mater Quality - DU B107 Page n ot~7? PE# TOPB1A Extramural Task: Accomplishments: (continued) FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 04 Develop, Analyze and Distribute Quality Control (QC) Samples for Water-related Analytes (continued). Chlorophyll (Spectrophotometry and Fluorometric), ATP, Reference Toxicants (cadmium chloride, sodium lauryl sulfate, and sodium pentachlorophenate), simulated plankton and natural plankton for counting, Algae for Identification (two samples), and five bacterial indicator cultures have been developed and 5,091 ampuls were distributed. A new reference toxicant, sodium pentachlorophenate, was produced. Several pure cultures and natural collections of algae for use in identification samples were obtained. A chlorophyll extract was prepared from natural periphyton to provide a source of chlorophyll £ in future samples. A new algae for sample identification was prepared. A new procedure involving high performance liquid chromatography (HPLC) analysis of algal pigments is being investigated, which provides information on several chlorophyll degradation products and other accessory pigments. A calibration sample for this HPLC analysis is also under development. Status: Annual Report on QC Sample Program Completed (12/85) ------- Page 6 of Project No. 04 APPROACH Water Quality - DU B107 Page 12 of /b PE# OTB1A OUTPUT Referee Analytical Services A. C. ORD Contact Name Harry Kolde FTS No. 684-7325 Resources B. R/D $5K $(000) 14.7 PFT 0.2 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 04 Extramural Task: Referee Laboratory Services. Purpose: Usage of large numbers and types of quality control (QC), performance evaluation (PE) and spiking/calibration samples in all USEPA programs to assess the quality of monitoring data necessitates that true or reference values associated with the samples are in fact, valid. Otherwise poor decisions will result which could adversely impact the environment. Therefore, referee laboratories are used to establish the veracity of all samples. Approach: Referee laboratories are selected through the competitive procurement process upon the basis of PE and cost for the analytes of interest. These analytes include trace metals, nutrients, minerals, sodium and corrosivity, demand, priority pollutants in samples designed for gas chromatograph (GC) and GC/mass spectrometer (MS), polychlorinated biphenyls (PCBs) in oil, and synthetic organic contaminants specified in the Clean Water Act and in the Consent Decree. Accomplishments: Referee laboratories conducted a total of 2,318 analyses: (1) 90 neat organic analyses to establish purity of materials in USEPA's Repository for Toxic and Hazardous Materials, (2) 1,876 analyses on QC and PE samples produced inhouse and on contract, (3) 320 analyses on spiking/calibration solutions from USEPA's Repository for Toxic and Hazardous Materials, (4) No analyses on neat surrogates related to USEPA Methods 624 and 625, and (5) analyses on 32 neat surrogate solutions. Status: Annual Report on Referee Analytical Services Completed (12/85) ------- Page 7 of Project No. 04 APPROACH Page 13 of 76 PE# MPB1A Water Quality - DU B107 C. ORD Contact OUTPUT Continue NBS Traceability Name John Winter A. FTS No. 684-7325 Resources B. R/D $20K $(000) 29.7 PFT 0.2 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 04 Extramural Task: Establish Traceability of Quality Control (QC) and Performance Evaluation (PE) Samples to National Bureau of Standards (NBS). Purpose: The QC and PE samples utilized throughout the United States and internationally in water/wastewater-related monitoring programs must be of high quality since they are involved in many important decisions. As such, there is a stringent quality assurance program to assure the veracity of the QC and PE samples including traceability to the NBS. Approach: An interagency agreement (IAG) was signed with the NBS to develop a protocol for traceability of QC and PE samples, and then to implement the protocol for those analytes/samples of interest to the Agency for which NBS has expert analytical capabilities. Accomplishments: NBS verified, thereby establishing traceability for pesticides (lindane, endrine and methoxychlor) for Water Supply (WS) Studies 19 and 20, two herbicides (2,4-D and Silvex), and 14 volatile organic contaminants (VOCs) (trans and cis 1,2-dichloroethylene, dibromo- chloropropane, o-dichlorobenzene, ethylbenzene, chlorobenzene, sytrene, toluene, xylene, ethylene dibromide, chloroform, bromodi- chloromethane, dibromochioromethane and bromoform). Seven sludges which are to be used in an interlaboratory method validation study are currently being analyzed. Status: Annual Report on Traceability to NBS Completed (12/85) ------- Page 8 of Project No. 04 Page 14 of 76 APPROACH PE# AAPB1A Water Quality - DU B107 C. ORD Contact OUTPUT Externalization of QA Programs. Name John Winter A. FTS No. 684-7325 ftesources B. R/D $ OK $(000) 9.7 PFT 0.2 OPFT PFTE OPFTE Inhouse Task: Purpose: Approach: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 04 Externalization of Quality Assurance (QA) Programs. Recover costs of production, distribution, and administration of quality control (QC) and performance evaluation (PE) sample programs associated with the drinking water, industrial waste, and water quality program. Promulgate a cost recovery rule for the preparation and distribution of QC and PE samples, set up a mechanism for collecting such fees through the USEPA Financial Management Office, and begin the externalization process for these sample types. Accomplishments: An externalization task force was formed of USEPA personnel from the Comptroller's Office; Office of General Counsel; Office of Program Management; Office of Acid Deposition, Environmental Monitoring and Quality Assurance (OADEMQA); operating program offices; the regional offices; and the three EMSL laboratories to study and recommend the best option for externalization of QA support services. Concur- rently, EMSL-Cincinnati prepared a white paper on costs for consideration by the Task Group. Discussions were also held between the Contracts Management Division and EMSL-Cincinnati to explore the best means to charge and collect user fees for these services and to expedite return of funds to EMSL-Cincinnati for maintenance of the QA program. Based on these deliberations and discussions, OADEMQA prepared a draft of a proposed rule: Proposed User Charges for Certain Quality Control and Performance Evaluation Samples Under the Clean Water Act and the Safe Drinking Water Act which was subsequently published in the Federal Register on September 16, 1986. Comments are due by October 31, 1986. Status: Report on the Externalization QA Program Completed (5/86) ------- Water Quality Research Committee Paqe 15 of 76 PE No. APTjTTT A. OUTPUT: Monitoring Measurements and Quality Assurance C. ORD Contact Reference Chemical Methods - Water and Name: J. J. Lichtenberq Sediment Analysis FTS No. 684-7306 B. RESOURCES: 3384.0 k FTE 7.0 FY 86 ANNUAL REPORT Project No. 05 Purpose and Approach The purpose of this project is to evaluate and standardize sample collection and chemical measurement methods for pollutants in water and sediments. In-house and under contract, single laboratory accuracy and precison data and method detection limits will be obtained for organic and metal analytes in environmentally contaminated water, sludge, sediment, and dredge material matrices using standardized extraction, cleanup and determination procedures and, when required, development of new techniques and procedures. Progress and Accomplishments Work on the project for "Identification and Determination of Metal Ions and Their Organometallic and Metal Chelate Compounds by High Performance Liquid Chromatography (HPLC)" continued throughout the year. A report, "Speciation of Inorganic and Organometallic Mercury by High-Performance Liquid Chromatography with Reductive Amperometric Electrochemical Detection", has been submitted for journal publication. It was submitted to the program office in May 1986. Investigations will continue in this area in FY 87 with the application of HPLC to 2-mercaptoethanol complexes of three organomercury compounds, i.e., methyl-, ethyl-, and phenylmercury. A special project to develop a method for acid soluble metals was completed this year. An overview of the technical findings resulting from the "Evaluation of Method 200.1 Determination of Acid Soluble Metals" was presented at the Society for Applied Spectroscopy (SAS) Seminar on Atomic Spectroscopy, April, 1986. An abridged version of a report on this topic was submitted to the U. S. Environmental Protection Agency (USEPA) Industrial Technology Division for incorporation into the proceedings of the Ninth Annual (1986) Analytical Symposium. The project to evaluate procedures for digestion and extraction of inorganic pollutants from biological fish tissue was begun in the second quarter. Initially, two techniques for extraction and solubilization of the tissue, microwave digestion and chemical treatment with tetramethylammonium hydroxide, are being investigated. A report on this project is planned for mid-FY 87. ------- Page of Project No. 05 Page 16 of 76 Work to develop methods for nonvolatile hazardous substances using a liquid chromatography/mass spectrometry (LC/MS) interface was begun early in FY 86. The unit connects the effluent from a HPLC to a Finnigan Model 4500 quadrupole mass spectrometer. Emphasis is on methods for carbamate, amide, urea, and triazine pesticides that are not amenable to gas chromatography/mass spectrometry (GC/MS) and for which no generic methods exist. This project is in the quantitative analysis stage including preliminary assessments of precision, accuracy, and detection limits. The project to develop design criteria for mechanical construction of a fiber optic chemical analyzer is continuing at Battelle Columbus. Analysis of the fiber optics technique determined that interferometry measurements of the sensitized fiber and the use of an elliptical fiber optics core provides the greatest sensitivity. However, since the system is extremely sensitive to temperature, compensatory techniques are being explored. In-house studies including electron microscope photographs of the fiber optics coated with 3-cyanopropyl silane showed excellent bondage and large surface area which should result in more sensitivity to polar compounds. ------- Industrial Wastewater Research Committee Page 17 of 76 PE No. BETO A. OUTPUT: New and Improved Analytical Test Procedures C. ORD Contact for Pollutants in Industrial Wastewater Name: J. J. Lichtenberg FTS No. 684-7306 B. RESOURCES: $638.6K FTE 10.1 FY 86 ANNUAL REPORT Project No. 06 Purpose and Approach The purpose of this project involves development of improved priority pollutant 600 series methods to correct deficiencies identified by users of the methods and to improve state-of-the-art flow measurement techniques. Liaison will be maintained with users of the methods to identify problem areas. A log of deficiencies will be maintained. These will be prioritized in order of seriousness and appropriate research will be initiated to correct the deficiencies. The methods will then be revised as appropriate. Progress and Accomplishments A continuing project to correct inadequacies of 304(h) methods for application to specific matrices is maintained. Inadequacies are being reviewed and appropriate action to modify methods is being taken. The Annual Report on these deficiencies is being prepared. Specific areas being addressed are as follow: Pesticide Methods - The proposed regulation to add new methods to Part 136 and move currently approved methods from Part 455 fell apart when the Agency decided to remand the Part 455 regulation. All methods approved there will now need to be reproposed in Part 136. A significant restructuring of the package is now required. Priority Pollutant Methods - The final rule of the October 26, 1984 interim rule was redrafted and forwarded again to Office of General Counsel (OGC) and the Work Group for comment, along with the final rule on the housekeeping proposal of that date, and the notice of data availability on June 30, 1986. Other Chemical Methods - The Virginia Edison Power Company (VEPCO) Settlement Agreement and nationwide alternate test procedure (ATP) for inductively coupled plasma (ICP) were approved by the Work Group at the annual meeting. All chemical methods previously proposed for Part 136 by the Industrial Technical Division (ITD) were withdrawn at the meeting. The Sampling and Field Measurements Section continues to provide technical assistance to the Underground Injection and Control (UIC) Program. A report on "Flow Measurements for the UIC Program - A Review" has been drafted and is undergoing technical and administrative review. ------- Page _2_ of Project No. 06 Page 18 of 76 The project to develop a Kriging program for sampling sediments using IBM-PC has been completed. A paper, "A Universal Kriging Program for the IBM-PC for use in Monitoring Sediments in Lakes", has been submitted for publication in the proceedings of the "Symposium on Chemical and Biological Characterization of Municipal Sludges, Sediments, Dredge Spoils and Drilling Muds", which was held in Cincinnati, Ohio, May, 1986. In the area of technical and engineering support in the use of computers, a draft report titled "Functional Requirements for the Single Laboratory Method Validation System on the IBM-PC" was delivered early in FY 86. The program is available in disk form and has been in great demand. More than 170 requests have been filled to date. Work on the organic accumulator project was halted during the 3rd quarter so that the principal investigator could devote full time to the evaluation of a wide-bore capillary column gas chromatography (GC) system employing the photoionization detector (PID) and electrolytic conductivity detector (ECD) in series for drinking water analyses. A new method (Method 680), that resulted from work performed during FY 85, was delivered to the program office early in FY 86. This method determines polychlorinated biphenyls (PCBs) and pesticides by degree of chlorination. ------- APPROACH Industrial Waste - DU B116 Page 19 of 76 PE# BEflC Verify and distribute quality control/performance OUTPUT evaluation samples and repository standards. A. C. ORD Contact Name Harold Clements FTS No. 684-7325 Resources B. $(000) 71.8 PFT 0.5 OPFT 1.0 PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 07 Inhouse Task: Develop Performance Evaluation (PE) Samples. Purpose: Provide a means for evaluating USEPA, USEPA contractor, state, and local laboratories analyzing samples as required under the Clean Water Act. Approach: As part of the Agency's quality assurance (QA) program, PE samples are designed, developed, produced, and verified by repeated analyses. Stable, homogeneous samples with known true values are prepared as concentrates and used to evaluate 700-900 USEPA, state, and local laboratories in formal semi-annual studies. Samples are also distributed on request from USEPA project officers to USEPA contractors. Accomplishments: PE samples were prepared for total phenolics (3,000 ampuls), total residual chlorine (6,000 ampuls), and mineral series (24,000 ampuls). Initial analyses of the samples verified the theoretical concen- trations. Final verification analyses were completed for all samples before distribution in Water Pollution (WP) Studies 16 and 17. Samples were sent to 546 laboratories in WP Study 16 and 830 laboratories in WP Study 17. Most of these laboratories partici- pated in both the organic and the inorganic portion of the studies. In total 73 analytes were each tested at two separate concentrations. Status: Annual Report on Design, Development, and Distribution of PE Samples Completed (12/85) ------- Page 2 of Project No. 07 Paqe 20 of 76 APPROACH PE# BEB1C Industrial Waste - DU B116 Verify and distribute quality control/performance C. 0RD Contact OUTPUT evaluation samples and repository standards. Name Paul Britton A. FTS No. 684-732$ Resources B. $(000) 59.1 PFT 0.2 OPFT 0.5 PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 07 Conduct Performance Evaluation (PE) Studies. Provide a system for evaluating the skills of USEPA, USEPA contractor, state, and local laboratories analyzing samples as required under the Clean Water Act. As part of the Agency's Mandatory Quality Assurance Program, PE samples are designed, developed, produced, and verified by repeated analyses. Stable, homogeneous sample concentrates with known true values are prepared and used in formal PE studies to evaluate 700-900 USEPA, state, and local laboratories in semi-annual studies. Samples are also distributed on request from USEPA project officers to USEPA contractors. Accomplishments: Two PE studies were conducted for USEPA, USEPA contractor, state, and local laboratories as nominated by the Regions and states. The 73 analytes tested at two concentrations included 21 trace metals, 12 minerals, 5 nutrients, 3 demand, 2 polychlorinated biphenyls (PCBs), 8 pesticides, 11 volatile organics, 6 aromatic purgeables, total cyanide, non-filterable residue, oil and grease, total phenolics, and total residual chlorine as analytes. Results were compared with acceptance limits based on previous study data and reports prepared for each laboratory. Performance in the studies identified problems for investigation and resolution. Samples were sent to 500-700 laboratories in each of the semi-annual studies conducted during February and August 1986. New samples were prepared for future studies in FY87 and beyond. In WP015, samples were sent to 726 laboratories of which 555 responded with data. Results were evaluated and reports sent on December 7, 1985. In WP016, samples were sent to 552 laboratories of which 437 returned data for evaluation. Results were evaluated and reports sent to participants on June 6, 1985. Inhouse Task: Purpose: Approach: Status: Individual Laboratory PE Reports Distributed to Participants in Study WP015 and WP016 Completed (7/86) ------- Page 3 of Project No. 07 APPROACH Industrial Waste - DU B116 Page 21 of 76 PE# BEB1C OUTPUT QA Sample Repository A. C. ORD Contact Name Harry Kolde FTS No. 684-7325 Resources B. R/D $19.25K $(000) 32.5 PFT 0.2 OPFT PFTE OPFTE FY86 ANNUAL REPORT Qua!ity Assurance Branch, EMSL-Cincinnati Project No.: 07 Extramural Task: Referee Laboratory Services. Purpose: The large numbers and types of quality control (QC), performance evaluation (PE) and spiking/calibration samples used in all USEPA programs to assess the quality of monitoring data necessitates that true or reference values associated with the samples are in fact, valid. Otherwise poor decisions will result which could adversely impact the environment. Therefore, referee laboratories are used to establish the veracity of all samples. Approach: Referee laboratories are selected through the competitive procurement process based on the PE and cost for the analytes of interest. These include trace metals, nutrients, minerals, sodium and corrosivity, demand, polychlorinated biphenyls (PCBs) in oil, fish and sediment, and all synthetic organic contaminants specified in the Clean Water Act and in the Consent Decree. Accomplishments: Referee laboratories conducted a total of 3,299 analyses: (1) 126 neat organic analyses to establish purity of materials in USEPA's Repository for Toxic and Hazardous Materials, (2) 2,669 analyses on QC and PE samples produced inhouse and on contract, (3) 472 analyses on spiking/calibration solutions from USEPA's Repository for Toxic and Hazardous Materials, (4) no analyses on neat surrogates related to USEPA Methods 624 and 625, and (5) analyses on 32 neat surrogate solutions. Status: Report on Referee Analytical Services Completed (12/85) ------- Page 4 of Project No. 07 APPROACH Industrial Waste - DU B116 Page n of 76 PE# IEE1C OUTPUT QA Sample Repository A. C. 0RD Contact Name Harry Kolde FTS No. 684-7325 Resources B. R/D $4K $(000) 13.6 PFT 0.2 OPFT PFTE OPFTE Extramural Task: Purpose: Approach: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 07 USEPA Repository for Toxic and Hazardous Materials, Produce, and Distribute Calibration Standards and Surrogates. The USEPA Repository for Toxic and Hazardous Materials provides spiking/calibration solutions of organic compounds in support of regulations under the Clean Water Act and Consent Decree for Priority Pollutants. Compounds of interest to the 304(h) and priority pollutant regulations are purchased or synthesized, then purified, dissolved in the appropriate solvent, and dispensed in 2 mL ampuls. The verity of pure compounds and concentration of the solutions in ampuls are verified by referee laboratories. Upon verification, spiking/cali- bration solutions are distributed to USEPA, USEPA contractor, state, and local laboratories engaged in monitoring the environment. Accomplishments: 1, Spiking/calibration solutions for all 110 organic priority pollutants under the Consent Decree are available for use by USEPA, USEPA contractor, regional, state, and local labora- tories. The remaining one is now being tested by referee laboratories for verity. 2. In FY86, 76,200 spiking/calibration solutions were distributed to 1925 USEPA, regional, state, and local laboratories engaged in environmental monitoring. Compounds available for distri- bution listed in USEPA Quality Assurance Newsletter were requested from the Quality Assurance Branch. 3. Of the 16 gas chromatograph/mass spectrometer (GC/MS) Surrogates specified in USEPA Methods 624 and 625, all are now available for use as calibration standards. 4. Native and l3C-labeled 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) are available as calibration standards. Status: Annual Report on Repository Completed (12/85) ------- Page 5 of Project No. 07 Page 23 of 7fi APPROACH PE# BEB1C Industrial Waste - DU B116 C. ORD Contact OUTPUT Continue NBS Traceability Name John Winter A. FTS No. 684-7325 Resources B. R/D $19.25 $(000) 32.5 PFT 0.2 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 07 Extramural Task: Establish Traceability of Quality Control (QC) and Performance Evaluation (PE) Samples to National Bureau of Standards (NBS). Purpose: The QC and PE samples utilized throughout the United States and internationally in water/wastewater related monitoring programs must be of the highest quality since they are involved in many important decisions by USEPA and the state agencies. As such, a stringent quality assurance program is needed to assure the veracity of the QC and PE samples; this program includes traceability to NBS. Approach: An interagency agreement (IAG) is maintained with the NBS to develop a protocol for traceability of QC and PE samples, and then to implement the protocol for those analytes and samples of interest to the Agency for which NBS has expert analytical capabilities. Accomplishments: NBS verified, thereby establishing traceability for trace pesticides (lindane, endrine and methoxychlor for Water Supply (WS) Studies 19 and 20, two herbicides (2,4-D and Silvex), and 14 volatile organic contaminants (VOCs) (trans and cis 1,2-dichloroethylene, dibromo- chloropropane, o-dichlorobenzene, ethylbenzene, chlorobenzene, sytrene, toluene, xylene, ethylene dibromide, chloroform, bromodi- chloromethane, dibromochloromethane and bromoform). Seven sludges which are to be used in an interlaboratory method validation study are currently being analyzed. Status: Annual Report on Traceability to NBS Completed (12/85) ------- Page 6 of Project No. 07 Paqe 24 of 76 APPROACH PE# BEB1C Industrial Waste - DU B116 C. ORD Contact OUTPUT QA Sample Repository Name Ed Berq A. FTS No. 684-7325 Resources B. R/D $19.25 $(000) 32.5 PFT 0.2 OPFT PFTE OPFTE Extramural Task: Purpose: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 07 Develop, Analyze, and Distribute Quality Control (QC) Samples £or Water-related Analytes. QC Samples are provided to USEPA, USEPA contractor, regional, state and local laboratories as a check on the technique and analytical methodology. Such checks are necessary to monitor the quality of data being generated in carrying out mandates of the Clean Water Act and Consent Decree for Priority Pollutants. Bionetics, Inc., the technical service contractor, develops, produces, and distributes QC samples. Development of new sample types requires: obtaining chemicals of the highest purity, a portion from the USEPA Repository for Toxic and Hazardous Materials, selecting the methodology for the compounds of interest, conducting retention time studies, combining groups of organic compounds to minimize overlapping gas chromatography peaks, and conducting 0, 45-, and 90-day stability studies. Those compounds remaining stable are produced at two concentration levels in lots of 3,000. Random samples are withdrawn during production and sent to referee labora- tories for verification analyses. Upon verification, the new samples are advertised in the USEPA Quality Assurance (QA) Newsletter and distributed to requesters. Approach: Accomplishments: 1, 4. Distribution of a total of 285,167 water pollution QC samples containing such analytes as trace metals for atomic absorption (AA) and inductively-coupled plasma (ICP) analyses, demands, nutrients, suspended solids, minerals, 109 priority pollutants for USEPA 600 series methodology, gas chromatograph/mass spectrometer (GC/MS) base neutrals, acids and purgeables, natural matrix samples such as polychlorinated biphenyls (PCBs) in oil and sediment, metals and pesticides in fish, phenols, cyanide, and crude oils. Sample types were advertised in the USEPA QA Newsletter and distributed on request to USEPA, USEPA contract, regional, state, and local laboratories. A total of 181,000 ampuls were produced to replenish depleted inventories and included such QC series as trace metals, cyanide, PCBs in oil and acetone, pesticides, demand, nutrients, and seven volatile organic series. Of the list of 188 industrial waste analytes, 136 are available as QC samples. Twenty-three QC series were verified as to true values, homogeneity, and stability by referee laboratories. Status: Report on QC Sample Program Completed (12/85) ------- Page 25 of 76 APPROACH PE# BEB1C Industrial Waste - DU B116 C. ORD Contact OUTPUT Externalization of QA Programs. Name John Winter A. FTS No. 664-7326 Resources B. R/D $ OK $(OOQ) 0 PFT 0 OPFT PFTE OPFTE Inhouse Task: Purpose: Approach: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 08 Externalization of Quality Assurance (QA) Programs. Recover costs of production, distribution, and administration of quality control (QC) and performance evaluation (PE) sample programs associated with the drinking water, industrial waste, and water quality program. Prepare a white paper on externalization of QA, promulgate a cost recovery rule for the preparation and distribution of QC and PE samples, set up a mechanism for collecting such fees through the USEPA Financial Management Office, and begin the externalization process for these sample types. Accomplishments: An externalization task force was formed of USEPA personnel from the Comptroller's Office; Office of General Counsel; Office of Program Management; Office of Acid Deposition, Environmental Monitoring and Quality Assurance (OADEMQA); operating program offices; the regional offices; and the three EMSL laboratories to study and recommend the best option for externalization of QA support services. Concur- rently, EMSL-Cincinnati prepared a white paper on costs, for consideration by the Task Group. Discussions were also held between the Contracts Management Division and EMSL-Cincinnati to explore the best means to charge and collect user fees for these services and to expedite return of funds to EMSL-Cincinnati for maintenance of the QA program. Based on these deliberations and discussions, OADEMQA prepared a draft of a proposed rule: Proposed User Charges for Certain Quality Control and Performance Evaluation Samples Under the Clean Water Act and the Safe Drinking Water Act which was subsequently published in the Federal Register on September 16, 1986. Comments are due by October 31, 1986. Status: Report on the Externalization QA Program Completed (5/86) ------- Page 2 of Project No. 08 APPROACH Industrial Waste - DU B116 Page 26 of 76 PE# BB1C Evaluate the performance of major NPDES discharger C. ORD Contact OUTPUT laboratories. Name Paul Britton A. FTS No. 684-7325 Resources B. $(000) 338.1 PFT 1.1 OPFT 0.4 PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 08 Extramural Task: Conduct Performance Evaluation (PE) Studies on Laboratories Producing Data Required under Major National Pollutant Discharge Elimination System (NPDES) Permits (Discharge Monitoring Report - Quality Assurance (DMR-QA) Studies). To provide an objective measure of how well laboratories can perform, which produce DMR data for major dischargers. With contract support, design and develop samples and conduct annual PE studies for the most frequently-occurring analytes in NPDES permits. Conduct a formal evaluation study on more than 7000 major dischargers for up to 29 analytes each. Use computerized data treatment to produce individual reports on each permittee and summary reports. Use contract computer specialists to maintain, improve, and expand the computer programs as necessary to support the NPDES Laboratory PE Studies. Effort made to maintain files of PE statistics and to use them to develop the best possible relationships between the true concentrations and statistical characteristics of analytical data. Statistical reports and services provided as needed. Accomplishments: Samples were made, verified, and shipped to 7383 major NPDES dischargers for DMR-QA Study 6. Data were returned by 6496 permittees for an 88% response, and individual PE reports were distributed by the end of August. The percentage of unacceptable data was lower than in any previous DMR-QA Study, continuing a trend of improvement with each successive study. Samples for three new analytes were added for DMR-QA Study 6 at the request of the Office of Water Enforcement and Permits: total cyanide, total phenolics, and total residual chlorine. Status: Development and Distribution of Necessary Study Materials to Regions, States, and Discharger Laboratories Final Report to each Participating Laboratory - Annual DMR-QA Study Purpose: Approach: Completed (5/86) Completed (11/86) ------- APPROACH Page 27 of 76 7T1 OUTPUT: Evaluation and Recommendation of Actions on ORD Contact NPDES Alternate Test Procedures NAME: Terence M. Grady FTS No. 684-7301 Resources: " B. $(000) 165.1 PFT 1.0 OPFT 0.7 PFTE OPFTE ANNUAL REPORT PROJECT NUMBER 09 Purpose and Approach The Equivalency Program is intended to encourage analytical methods development or improvement by the regulated community and by manufacturers of pollution measuring instruments. These alternate test procedures (ATPs) may be approved for case-by-case or nationwide use as mandated by 40 CFR Parts 136.4 and 136.5. After receipt of unsolicited ATP applications, necessary external and/or internal technical reviews are conducted and coordinated to provide a technically sound recommendation on approval or denial of the proposed ATP. Items considered during review include: availability of a well documented test procedure, docu- mentation of the applicability of the proposed procedure, performance character- istics such as accuracy, precision, and method detection limits, and equivalency data to an approved test procedure. Progress and Accomplishments During FY86, a total of 51 requests for approval of ATPs were received. Ten of the requests were for nationwide approval and the remaining 41 were for limited use. Quarterly and annual ATP reports were distributed to the Regional and Headquarters staff. The direct current plasma atomic emission spectroscopy method for metals was recommended for nationwide compliance monitoring use. The following table summarizes the applications received by this office and the actions recommended: National Pollutant Discharge Elimination System (NPDES): 51 a. Nationwide: 10 b. Limited Use: 41 c. Action Taken: 1. Recommended Approval: 19 2. Recommended Disapproval: 6 3. Non-Germane (Not ATP): 4 4. Requested Further Data: 19 5. Pending: 3 ------- Page 28 of 76 APPROACH PE# BLC1A Drinking Water - DU C104 Produce and distribute performance evaluation (PE) C. ORD Contact OUTPUT samples for water supply laboratory certification Name Harold Clements A. program. FTS No. 684-7325 B. $(000) 237.4 PFT 3.7 OPFT PFTE OPFTE Approach: Accomplishments: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 10 Performance Evaluation (PE) Studies for Certification. Under the Safe Drinking Water Act (SDWA) and the National Interim Primary Drinking Water Regulations (NIPDWR) and amendments, acceptable performance in PE studies is an annual requirement for certification of drinking water laboratories. In response to this need, the Quality Assurance (QA) Branch develops and provides sample series for each maximum contaminant level (MCL) analyte, and for monitoring analytes, listed in the primary drinking water regulations and amendments. New series samples are designed, prepared and verified by analyses, for each semi-annual study of approximately 1000 laboratories. Each study covers 22 analytes at two separate concentrations each. Over the past year the following ampuls were produced for future studies: nitrate/fluoride (12,000 ampuls), sodium/corrosivity (5,000 ampuls), volatile organics (6,000 ampuls), residual free chlorine (3,000), and trace metals (12,000). The ampuls were analyzed originally to verify the true concen- tration and then by the QA Branch and the referee laboratories to confirm homogeneity and stability over time. In Water Supply (WS) Study 18, 1113 laboratories were sent samples for testing 38 parameters/analytes, most at two concentrations. In WS Study 19, 911 laboratories were sent samples for certification. In the past year, 31 of the new volatile organic chemicals (VOCs), and 1445 compounds have been included in the studies. Status: Design, Develop^and Prepare Performance Evaluation Samples for Drinking Water Certification Program Completed (12/85) ------- Page 2 of Project No. 10 APPROACH Drinking Water - DU CI04 Page 29 of j£_ PE# BTC1A OUTPUT Quality Control/Performance Evaluation A. C. ORD Contact Name Harry Kolde FTS No. 684-7325 Resources B. R/D 80.4 $(000) 86.4 PFT 0.1 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 10 Extramural Task: Develop USEPA's Repository for Toxic and Hazardous Materials. Purpose: Approach: The USEPA Repository for Toxic and Hazardous Materials provides spiking/calibration solutions of organic compounds in support of regulations under the Safe Drinking Water Act and those contaminants specified in the Drinking Water Strategy Document. Compounds of interest to the Drinking Water Program are purchased or synthesized, purified, dissolved in an appropriate solvent, and dispensed in 2 mL ampuls. The verity of pure compounds and concentration of the compound in the ampul are verified by referee laboratories. Upon verification, spiking/calibration solutions are advertised in the Quality Assurance Newsletter and distributed to USEPA, USEPA contractor, state, and local laboratories engaged in monitoring the environment. Accomplishments: 1, Distributed 75,200 spiking/calibration solutions to 1930 USEPA, state, and local environmental laboratories engaged in monitoring. Compounds available for distribution listed in USEPA Quality Assurance Newsletter are requested from the Quality Assurance Branch, EMSL-Cincinnati. All organic analytes specified in National Interim Primary Drinking Water (NIPDW) regulations are available as certified calibration standards. Of the 126 organic analytes specified in the various Drinking Water regulations and Strategy Documents, 90 are certified for distribution as calibration standards. All of the volatiles and herbicides listed in the November 1985 Drinking Water regulations are now stocked as neats. Status: Annual Report on Repository Completed (12/85) ------- Page 3 of Project No. 10 Page 30 of 76 APPROACH PE# "BCClA Drinking Water - DU CI04 Produce and distribute quality control (QC) and C. ORD Contact OUTPUT performance evaluation (PE) samples for water supply Name Ed Berg A . laboratory certification program. FTS No. 684-7325 Resources B. R/D $45 $(000) 51 PFT 0.1 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 10 Extramural Task: Develop and Distribute Quality Control (QC) Samples. Purpose: Approach: Status: QC Samples are provided to USEPA, regional, state, and USEPA contractors as a check on analyst technique and analytical methodology. Such checks are necessary to insure that high quality data are being generated in carrying out mandates of the Safe Drinking Water Act. Bionetics, Inc., the technical service contractor, develops, produces, and distributes QC samples. Development of new sample types requires: obtaining chemicals of the highest purity from best purity sources such as the USEPA Repository for Toxic and Hazardous Materials, selecting the methodology for the compounds of interest, conducting retention time studies, combining groups of organic compounds to minimize overlapping gas chromatography peaks, and conducting 0, 45-, and 90-day stability studies. Those compounds proven stable are produced at two concentration levels in lots of 3,000. Random samples are withdrawn during production and sent to referee laboratories for verification analyses. Upon verification, new samples are advertised in the USEPA Quality Assurance Newsletter and distributed to requesters. Accomplishments: 1. Distributed 55,074 drinking water QC samples to USEPA, USEPA contractor, state, and local laboratories. Analytes included pesticides, herbicides, residual chlorine, turbidity, trihalo- methanes, trace metals for atomic absorption (AA) and inductively-coupled plasma (ICP) analytical procedures, nitrate/fluoride, and corrosivity. 2. Produced the following analyte groups to replenish depleted inventories: sodium/corrosivity and residual free chlorine. A total of 22,200 ampuls were produced. 3. Conducted stability testing on 14 QC series (pesticides, metals, and volatiles). Annual Report on QC Samples Completed (12/85) ------- Page 4 of Project No. 10 Paqe 31 of 76 APPROACH PE# BLC1A Drinking Water - DU CI04 C. URD Contact OUTPUT Quality Control/Performance Evaluation Name John Winter A. FTS No. 684-7325 Resources B. R/D $30K $(000) 36 PFT 0.1 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 10 Extramural Task: Establish Traceability of Quality Control (QC) and Performance Evaluation (PE) Samples to the National Bureau of Standards (NBS). Purpose: The QC and PE samples utilized throughout the United States and internationally in water-related monitoring programs must be of the highest quality since they are involved in many important decisions. As part of a stringent quality assurance program to assure the veracity of the QC and PE samples, traceability to NBS is established. Approach: An interagency agreement (IA6) was signed with NBS to develop a protocol for traceability of Drinking Water related QC and PE samples, and then to implement the protocol for top priority samples of interest to the Agency and those for which NBS has expert analytical capabilities. Accomplishments: NBS verified concentrations, thereby establishing traceability for pesticides (lindane, endrine and methoxychlor) for Water Supply (WS) Studies 19 and 20, two herbicides (2,4-D and Silvex), and 14 volatile organic contaminants (VOCs) (trans and cis 1,2-dichloro- ethylene, dibromochloropropane, o-dichlorobenzene, ethylbenzene, chlorobenzene, sytrene, toluene, xylene, ethylene dibromide, chloroform, bromodichloromethane, dibromochloromethane and bromoform). Status: Annual Report on Traceability to NBS Completed (12/85) ------- Page 5 of Project No. 10 APPROACH Drinking Water - DU CI04 Page 32 of 76 PE# BLClA OUTPUT Quality Control/Performance Evaluation A. C. ORD Contact Name Harry Kolde FTS No. 684-7325 Resources B. R/D $9.5 $(000) 15.5 PFT 0.1 0PFT PFTE 0PFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 10 Extramural Task: Conduct Verification Analyses on all performance evaluation (PE)/quality control (QC) Samples. Purpose: Usage of large numbers and types of QC, PE and spiking/calibration samples in USEPA programs to assess the quality of monitoring data necessitates that true or reference values associated with the samples are in fact, valid. Otherwise poor decisions could result which would adversely impact the environment. Referee laboratories are used to establish the veracity of all samples. Approach: Referee laboratories are selected through the competitive procure- ment process upon the basis of a PE study and competitive cost for the analytes of interest. These include trace metals, nutrients, minerals, sodium and corrosivity, demand, priority pollutants in samples designed for gas chromatograph (GC) and GC/mass spectrometer (MS), polychlorinated biphenyls (PCBs) in oil and fish, synthetic organic contaminants specified in the Drinking Water Strategy Document, and for other analytes regulated by the Agency. Accomplishments: Referee laboratories conducted: (1) 90 neat SOC analyses to establish purity of materials in USEPA's Repository for Toxic and Hazardous Materials, (2) 3,199 analyses on QC and PE samples produced inhouse and on contract, (3) 320 analyses on spiking/ calibration solutions from USEPA's Repository for Toxic and Hazardous Materials, (4) No analyses on neat surrogates related to USEPA Methods 624 and 625, and (5) analyses on 32 spiking/ calibration solutions for surrogate compounds related to USEPA Methods 624 and 625. Status: Annual Report on Referee Analytical Services Completed (12/85) ------- Page 6 of Project No. 10 Page 33 of 76 APPROACH PE# BLC1A Drinking Water - DU C104 C. ORD Contact OUTPUT Externalization of QA Programs. Name John Winter A. FTS No. 684-7325 Resources B. R/D $ OK $(000) 0 PFT 0 OPFT PFTE OPFTE Purpose: Approach: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 10 Inhouse Task: Externalization of Quality Assurance (QA) Programs. Recover costs of production, distribution, and administration of quality control (QC) and performance evaluation (PE) sample programs associated with the drinking water, industrial waste, and water quality program. Promulgate a cost recovery rule for the preparation and distribution of QC and PE samples, set up a mechanism for collecting such fees through the USEPA Financial Management Office, and begin the externalization process for these sample types. Accomplishments: An externalization task force was formed of USEPA personnel from the Comptroller's Office; Office of General Counsel; Office of Program Management; Office of Acid Deposition, Environmental Monitoring and Quality Assurance (OADEMQA); operating program offices; the regional offices; and the three EMSL laboratories to study and recommend the best option for externalization of QA support services. Concur- rently, EMSL-Cincinnati prepared a white paper on costs and other considerations for the Task Group. Discussions were also held between the Contracts Management Division and EMSL-Cincinnati to explore the best means to charge and collect user fees for these services and to expedite return of funds to EMSL-Cincinnati for maintenance of the QA program. Based on these deliberations and discussions, OADEMQA prepared a draft of a proposed rule: Proposed User Charges for Certain Quality Control and Performance Evaluation Samples Under the Clean Water Act and the Safe Drinking Water Act which was subsequently published in the Federal Register on September 16, 1986. Comments are due by October 31, 1986. Status: Report on the Externalization QA Proqram Completed (5/86) ------- Drinking Water Research Committee Page 34 of 76 PE No. BnOT" A. OUTPUT: Improved and Validated Organic Analytical C. ORD Contact Methods for Drinking Water Name: J. E. Lonqbottom FTS No. 684-7308 B. RESOURCES: % 84.OK FTE 2.0 FY 86 ANNUAL REPORT Project No. 11 Purpose and Approach The purpose of this project is to provide new, improved or, alternate analytical methods for monitoring synthetic organic chemicals in drinking water. Sample concentration techniques, capillary column gas chromatography (GC), GC-mass spectrometry (MS), and high performance liquid chromatography (HPLC) methods will be investigated. Progress and Accomplishments Methods for Volatile Organic Chemicals (VOCs) - Methods 502.1, 503.1, 504, and 524.1 were modified to reflect public comment on the proposed VOCs maximum contaminant levels (MCLs) and monitoring requirement. The principal changes to the methods at this time involved reduction of the scope of Method 524.1 to reflect conventional packed column analytical practices and strengthening the identification criteria in this method to reduce false positives. Two compounds were deleted from the scope of all purge and trap methods due to reactivity (pentachloroethane) or poor purging efficiency bis (2-chloro- isopropyl ether). The quality control (QC) section of all methods was tightened to focus on control near the method detection limit. The revised manual was forwarded to the Office of Drinking Water (ODW) in September. Future plans are to incorporate synthetic organic chemical (SOC) methods into the manual. Reference Methodology for SOCs - Method 524.2 - A capillary column method, including both wide-bore and conventional fused silica capillary column (FSCC) technique, suitable for determination of the volatile VOCs, "1445" compounds, and volatile SOCs with a single analysis was forwarded to ODW in September. Method 502.2 - A capillary column (wide-bore) method for volatiles using the Hall and photoionization detector (PID) detector in series was drafted based upon in-house work. As with the GC/MS method (524.2), the new method shows excellent precision and sensitivity. It is scheduled for completion in October. Method 505 - A micro-extraction method for organochlorine pesticides, polychlorinated biphenyls (PCBs), and the SOC, alachlor, was completed and forwarded to ODW in September. The method offers substantial savings in analytical costs, if it is sensitive enough to measure MCLs for these contaminants. ------- Page 2 of Project No. 11 Page 35 of 76 Method 515 - A FSCC update of the electron capture derivatization method for phenoxyacid herbicides was forwarded to ODW in September. The method has been optimized for the chlorophenoxy acids on the SOC list and for pentachloro- phenol. GC/MS Methods for Pesticides and PCBs - A capillary column method is being developed for application to selected SOC pesticides. Work this quarter centered around choosing selected ion monitoring (SIM) parameters for the analysis of these SOCs. Method range studies for these compounds for both the full scan mode and the SIM mode were completed but no methods write-up was prepared pending further ODW guidance. Method for Acrylamide - Decomposition of the synthesis product, dibromo- propioamide, has slowed development of a method for this compound. Instability and anomalies in GC have led to a redirection toward understanding the reactions of acrylamide with chlorine in water. Work on this method is expected to continue for, at least, another six months. Analytical Methods for the National Groundwater Pesticides Survey - A total of five broad spectrum methods, and a sixth method specifically for ethylene thiourea (ETU) have been drafted. Revision of the methods to incorporate final data and peer review comments continued through September and should be completed in October. Two methods (507, Nitrogen/Phosphorus Pesticides and 508, Organochlorine Pesticides) were forwarded to ODW in September to support the SOC proposal. Analytical Methods for Disinfection By-Products—Work was conducted to test the most promising analytical approach for chlorinated acetic acids. A modification of Method 515 appears to be suitable for these compounds. Work on this project will be accelerated in the next quarter. ------- APPROACH Page 36 of 76 J~. OUTPUT: Evaluation of Alternate Test Procedures to uku contact Meet Requirements of the Safe Drinking Water NAME: Terence M. Grady Act FTS No. 684-7301 Resources: B. $(000) 50.0 PFT 1.0 OPFT PFTE OPFTE ANNUAL REPORT PROJECT NUMBER 12 Purpose and Approach The Equivalency Program is intended to encourage analytical methods development or improvement by the regulated community and by manufacturers of pollution measuring instruments. These alternate test procedures (ATPs) may be approved for case-by-case or nationwide use as mandated by 40 CFR Part 141.27. After receipt of unsolicited ATP applications, necessary external and/or internal technical reviews are conducted and coordinated to provide a technically sound recommendation on approval or denial of the proposed ATP. Items considered during review include: availability of a well documented test procedure, docu- mentation of the applicability of the proposed procedure, performance character- istics such as accuracy, precision, and method detection limits, and equivalency data to an approved test procedure. Progress and Accomplishments During FY86, a total of 23 requests for approval of ATPs were received. Five of the requests were for nationwide approval. The remaining 18 were limited-use requests. Quarterly and annual ATP reports were distributed to the regional and Headquarters staff. As a result of the comparability data submitted by the J. T. Baker Chemical Company, approval for the use of solid phase extraction columns for pesticides was recommended. The following table summarizes the applications received by this office and the actions recommended: National Interim Primary Drinking Water Regulations (NIPDWR): 23 a. Nationwide: 5 b. Limited Use: 18 c. Action Recommended: 1. Recommended Approval: 15 2. Recommended Disapproval: 0 3. Non-Germane (Not ATP): 2 4. Requested Further Data: 5 5. Pending: 1 ------- APPROACH Page 37 of j£_ PE# BK1A Drinkinq Water - DU C104 C. ORD Contact OUTPUT Method Validation Study Name Harold Clements A. FTS No. 684-7325 Pp^nnrrpc B. $(000) 0 PFT 0 OPFT PFTE OPFTE Inhouse Task: Purpose: Approach: Accomplishments: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 13 Conduct Method Validation Study for Maximum Trihalomethane Potential (MTP). Verification of USEPA Method 510.1 with bias and precision data. Produce performance evaluation samples and develop collaborative study to produce data to support the use of the USEPA Method 510.1. Samples were designed and produced to conduct a formal method validation study for MTP (USEPA Method 510.1). Samples were distributed in the second quarter of FY85 and data returned to the Quality Assurance (QA) Branch in the third quarter. The necessary statistical calculations were completed and the report written. Status: Final Report for MTP Method Validation Study Completed (9/86) ------- Page 2 of Project No. 13 Page 38 of 76 APPROACH PE# EOTlA Drinking Water - DU CI04 C. ORD Contact OUTPUT Method Validation Study Name Ray Wesselman A . FTS No. 684-7325 Resources B. R/D $700K $(000) 741.7 PFT 1.0 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 13 Extramural Task: Method Validation Studies for Volatile Organic Chemicals (VOCs), Synthetic Organic Chemicals (SOCs), and Section 1445 Organic Chemicals. Purpose: In support of the Safe Drinking Water Act (SDWA), interlaboratory method validation studies (IMVS) are conducted for USEPA methods for the purpose of establishing bias/recovery, precision, and other statistics. Approach: MVSs are conducted by a prime contractor involving 10 contract laboratories. The prime contractor provides three Youden pairs of ampul concentrates containing the compounds specified. The participating laboratories spike the concentrates of analytes into water types and analyze the sample according to the USEPA method. Analytical data are processed with USEPA's IMVS computer program which provides regression equations for bias and precision and other statistics. Accomplishments: A request for proposal (RFP) was developed to obtain 10 participants in an IMVS for 8 drinking water methods which included VOCs, SOCs, and 1445 organics. Offerors' proposals were evaluated and those judged technically acceptable were sent performance evaluation (PE) samples to confirm laboratory capabilities. Contracts will be awarded in October 1986 with the IMVS commencing shortly thereafter. Status: Status Report on the IMVS for VOCs, SOCs, and Section 1445 Compounds On Schedule (9/«7) ------- APPROACH Drinking Water - DU C104 page 39 ot 2JL_ PE# TJLC1A Produce and distribute microbiological performance OUTPUT evaluation samples for water supply laboratory A. certification program. C. ORD Contact Name Gary Collins FTS No. ' 684-7325 R6S0urc6S B. $(000) 18.3 PFT 0.4 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 14 Development and Preparation of Microbiological Performance Evaluation (PE) Study Samples for Certification. Under the Safe Drinking Water Act (SDWA) and the National Interim Primary Drinking Water Regulations (NIPDWR) and amendments, acceptable performance in PE studies is an annual requirement for certification of drinking water laboratories. In response to this need, the Quality Assurance (QA) Branch develops and provides sample series for each maximum contaminant level (MCL) analyte, and for monitoring analytes, listed in the primary drinking water regulations and amendments. Approach: Vials of lyophilized coliform organisms are designed, prepared and verified by analyses. Each semi-annual study of approximately 100 laboratories is conducted using these cultures. Accomplishments: Samples for studies WSM07 and WSM08 (concurrent with WS017 and WS018) for total coliforms were completed and Study WSM09 initiated. Task: Purpose: Status: Develop and Prepare Coliform Samples for WSM07 and WSM08 Completed (7/86) ------- Page 2 of Project No. 14 Page 40 of 76 APPROACH PE# BLC1A Drinking Water - DU C104 Conduct semi-annual performance evaluation studies C. ORD Contact OUTPUT for chemical and microbiological analysis of Name Paul Britton A. drinking water. FTS No. 684-7325 Resources B. $(000) 45.7 PFT 2.0 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 14 Conduct Water Supply (WS) Laboratory Performance Evaluation (PE) Studies. To provide an objective basis for evaluating drinking water laboratory performance for certification, under National Interim Primary Drinking Water Regulations (NIPDWR) of the Safe Drinking Water Act (SDWA). Laboratories that have applied for, or currently have, USEPA Drinking Water Laboratory Certification, are required to participate annually in PE studies for each analyte to be certified, and to perform satisfactory. PE samples cover 8 trace metals, nitrate, fluoride, 4 pesticides, 2 herbicides, 4 individual and total trihalomethanes, turbidity, free residual chlorine, and total coliforms at two concentration levels each, as well as one level for sodium and corrosivity analytes. USEPA compares the analytical results from each laboratory against acceptance limits generated from the known true concentrations and results from the current and past studies. Laboratories performing unacceptably or missing the primary study can participate in a second (follow-up) study each year. Laboratories performing acceptably in one study each year are eligible for USEPA certification. Accomplishments: WS-PE study reports were generated for studies WS017 and WS018, with 713 and 945 participating laboratories, respectively. Study WS019 was initiated and is to be completed next year. WSM07 and WSM08 microbiological samples were shipped to approximately 100 USEPA and state laboratories at the same time as other WS study samples. The laboratories reported the microbiological data separately, but final study reports covered all data reported. During the studies this year, special PE samples containing 20 new volatile organics (VOCs) were provided at two levels each for voluntary analyses to provide the Office of Drinking Water (ODW) with background information on these compounds considered for regulation but not for certification. VOC samples for other volatile organics will be added for voluntary analysis in all future studies. Status: Individual Laboratory PE Reports Distributed to Completed Participants in Study WS017, WS018, WSM07, and (9/86) WSM08. Task: Purpose: Approach: ------- Drinking Water Research Committee Page 4} of 76 PE No. BNTTiA" A. OUTPUT: Laboratory Certification Program for Drinking Water Quality Assurance C. ORD Contact Name: J. J. Lichtenberq FTS No. 684-7306 B. RESOURCES: % 455.7K FTE 6.0 FY 86 ANNUAL REPORT Purpose and Approach Project No. 15 The purpose is to evaluate regional laboratories and personnel for capability to provide quality data in support of the National Interim Primary Drinking Water Regulations (NIPDWR) monitoring program, to approve regional labora- tories to do the required analyses, and to certify the regional staffs. This will be accomplished by review of the regional certification program and laboratory performance records and on-site evaluation of the regional labora- tories. Progress and Accomplishments Laboratory Certification Courses - Annual laboratory certification courses were prepared and conducted for chemistry and microbiology during the month of June. These courses provided the regional/state chemists and microbiologists the opportunity to become officially certified and be responsible for conduct- ing on-site audits of state and local laboratories requesting certification under the Safe Drinking Water Act 1974 (SDWA). All regional requests were met and, with only a few exceptions, the states' requests and overall needs were satisfied. These courses were presented by the Environmental Monitoring and Support Laboratory - Cincinnati (EMSL-Cincinnati) staff with able assistance from professional staff of the Technical Support Division, Office of Water. Plans are to offer these two courses again in FY 87. Annual Review of Regional Activities - Close liaison was maintained with the regions through key contacts with the regional Quality Assurance Officers (QAOs) and Drinking Water Representatives. Our laboratory QAO and Quality Assurance Management Staff (QAMS) representative actively participated with regional and program office representatives in developing and implementing QA techniques at the regional/state level. On-site visits were made to Regions 4, 5, and 6. The United States Geological Survey (USGS) laboratory in Denver, Colorado was evaluated for compliance with Drinking Water regulations on April 15-17. This was done at the request of Regions 2 and 8. The USGS laboratory can be certified for inorganic and organic analysis of drinking water. Plans are being made to begin the next round of regional visits during the second half of FY 87. Eight regional on-site evaluation reports for state labora- tories were reviewed in FY 86. These were discussed with appropriate regional personnel and approved for distribution and subsequent certification actions. Review of four additional reports are pending. ------- Page _2_ of Project No. 15 Page 42 of 76 The Equivalency Program processed twenty-three (23) requests for approval of alternate test procedures. Eighteen (18) of these were for limited use and five (5) were for nationwide approval. Conduct Performance Evaluation (PE) Studies - WS017 and WS018, PE studies involving greater than 1000 laboratories each, were conducted in FY 86 for all chemical maximum contaminant levels (MCLs) and control analytes. The chemical sample concentrates were prepared, instructions written, PE samples distributed as unknowns. Data were returned to the QA Branch for processing and preparation of reports for each laboratory. Reports were sent to the participants and copies to the respective regional QAOs for any follow-up actions. WSM07 and WSM08, PE Studies for microbiological MCLs, for total coliforms were also completed for certification of USEPA and state laboratories in FY 86. Analyze Trends in PE Sample Program and Provide Performance Criteria - Updated statistics are provided on total analyses and method-by-method for Water Supply (WS) Studies WS017 and WS018 to Maria Gomez-Taylor of the ODW. As a special project, a computer program is being developed to summarize USEPA, state, and "all" laboratory performances in WS PE studies over the past years so as to identify those missing one or more analytes (exceeding acceptance limits) in two and in three successive studies, on an analyte-by-analyte basis. Generalized statistical estimates for each MCL contaminant (analyte) are also provided. These stated the mean recoveries and standard deviations of each analyte as a percentage of the MCL based on PE study data. Analytes included the current MCLs and the nine proposed volatile organic chemicals (VOCs). Preparation and Distribution of Known Quality Control (QC) Samples, Calibra- tion Standards and Unknown PE Samples for all Regulated Contaminants - All VOC analytes specified in proposed revision of the primary drinking water regula- tions are now available as certified calibration standards. Of the 126 analytes, VOCs and synthetic organic chemicals (SOCs) specified in the Drinking Water Strategy, 90 are certified for distribution as calibration standards. Over 75,000 calibration standards were distributed by EMSL-Cincinnati to USEPA laboratories, contractors/grantees, state, and local laboratories engaged in environmental monitoring. EMSL-Cincinnati distributed over 55,000 drinking water QC samples to USEPA regional, state, local, and USEPA contractor laboratories. Analytes included pesticides, herbicides, residual chlorine, turbidity, trihalomethanes, trace metals, nitrate, fluoride, corrosivity, Temik, and the new VOCs proposed for regulation. Provide Technical Assistance - Numerous telephone requests were handled directly by technical staff on matters related to chemical and microbiological methods usage, and to QA requirements/usage under the SDWA. In addition, specialized laboratory analyses were provided to the regions and states for uranium, gross alpha/beta, radium-226, and radium-228. ------- Page 3 of Project No. 1^ Page 43 of 76 Revision of the Drinking Water Certification Manual was begun at the request of the Office of Drinking Water (ODW). EMSL-Cincinnati has eight staff members serving in various capacities on the Committee, including Chairmanships of the Implementation and Analytical Methods and Quality Control Committees, Analytical Chemistry Methods Work Group and as members of the Steering Committee. Two steering committee meetings were attended at USEPA headquarters. The Analytical Chemistry and Microbiology Work Groups have held several meetings. Two of these included non-USEPA (state) members. The second drafts of these revised chapters have been transmitted to ODW for review. ------- Drinking Water Research Committee Page 44 of 76 PE No. BlCIF A. OUTPUT: Standardized and Validated Radiochemical C. ORD Contact Methods for Analysis of Drinking Water Name: 6. D. McKee FTS No. 684-7372 B. RESOURCES: % 130.5K FTE 3.0 FY 86 ANNUAL REPORT Project No. 16 Purpose and Approach The purpose of this project is to evaluate and modify as necessary procedures for radiochemical analysis of drinking water and to provide analytical technical assistance to the Office of Drinking Water (ODW). Methods for radium, uranium, and radon will be investigated. Up to 1176 survey samples will be analyzed. Progress and Accomplishments National Inorganics and Radionuclides Survey (NIRS) - Four-hundred and seventy-five (475) samples for 37 elements totaling 22,191 analyses were completed by inductively coupled plasma (ICP) this quarter. To verify the sample analyses, an additional 8869 quality control (QC) analyses also were completed. A total of 1176 samples were received for the NIRS project. No additional samples are expected. The table below provides a summary of samples received and analyses completed to date. Samples Samples Samples Completed QC Samples Analysis Received Started Completed This Quarter This Quarter Radon 1176 1176 1176 80 Uranium 1176 1176 1176 73 7 Gross A/B 1176 1176 1176 70 9 Ra-226 1176 1173 1128 86 12 Ra-228 1176 1144 1050 84 12 A summary report on this work was prepared and forwarded to the NIRS manager in September. The following technical assistance was provided in the area of radiochemistry and other drinking water related problems: o Four samples received by the Water Engineering Laboratory of Pima County Health Department, Arizona were analyzed for uranium, gross alpha and beta. o Five Ra-226 and 15 uranium analyses were performed for the Inorganics and Particulates Control Branch, Drinking Water Research Division for the pilot study for removal of radium at Lamont, Illinois. Ten analyses for Ra-226, five Ra-228, and 10 gross alpha and beta were performed at the request of the same division for the project to evaluate removal and waste disposal at Redhill Forest Development in Colorado. ------- FY 86 OUTPUT PLAN MICROBIOLOGY SECTION, BMB, EMSL-CINCINNATI DRINKING WATER - MONITORING SYSTEMS AND QUALITY ASSURANCE Page 45 of 76 PE* Zm OUTPUT Coliform Analysis - Drinking Water - Quality Assurance ORD Contact Name R. Bordner FTS No. 684-7319 Resources: $(000) 55.2K PFT 1^0 OPFT 0.0 PFTE UO OPFTE 0.0 Project 17 ANNUAL REPORT - FY 86 The final report on the comparison of the hydrophobic grid membrane filter (HGMF) procedure and standard membrane filter (MF) methods for coliform analysis was forwarded to the Office of Drinking Water and submitted to the Journal of Applied and Environmental Microbiology for publication. No significant differences were found between results from the standard MF and the HGMF. An interim report, "Development and Evaluation of an Alternative Total Coliform Membrane Filter Medium," was prepared, peer reviewed, and forwarded to the client program offices. The candidate and standard media, ranked in order of verified coliform recovery, were m-TECM, m-LSB, m-T7, m-Endo, and m-HAB. m-TECM and m-T7 were developed through cooperative agreements with the University of Rhode Island and Montana State University respectively, m-HAB was developed inhouse, m-LSB is a British medium, and m-Endo is the standard test medium. In a collaborative test of four media, m-TECM, m-T7, m-HAB, and m-Endo, by 23 laboratories from many different geographical areas analyzing local samples, a statistical evaluation showed no significant difference among the media. Plans were made for additional testing of lyophi1ized natural samples to be shipped to and analyzed by all participating laboratories. The statistical analyses of the data from the project to determine the precision and accuracy of the MF and most probable number (MPN) total coliform procedures were completed and an interim report entitled "Precision and Relative Accuracy of the Membrane Filter and Most Probable Number Total Coliform Methods Used for Drinking Water Analysis" was prepared. There was a significant difference between the precision of the two methods when natural samples were analyzed. Using the ASTM method for determining relative accuracy, the MF test was more accurate than the MPN method when the 23% positive bias of the latter was removed. Microbiologists participated in on-site visits to the Environmental Services Division, Region 3, Wheeling Office, and Regions 5 and 6, to determine compliance with drinking water laboratory certification requirements. ------- Page 2 of Project No. 17 Page 46 of 76 A training course entitled, "Drinking Water Laboratory Certification for Microbiology," was attended by 20 laboratory certification officers from USEPA regions, states, and territories. A paper entitled "Reliable Data Begin with Well-Planned Sampling Procedures," was presented March 23 at a workshop on "New Developments in Drinking Water," sponsored by the Board of Education and Training of the American Society for Microbiology. The final report by Drexel University on the application of the Presence- Absence (P-A) test in small water systems was sent out for peer review. The P-A test gave equivalent or better recovery of total coliforms from drinking water. The University presented a poster on "The Effects of Water Quality Parameters on Coliform Detection by Clark's P-A Test," at the Annual Meeting of the American Society for Microbiology, March 26, 1986, and a report on "Comparison of Clark's P-A Test and the Membrane Filter Method for Coliform Detection in Potable Waters," was published by the Journal of Applied and Environmental Microbiology. The results from the research by McNeese State University (MSU) and Florida International University (FIU) to determine sample holding effects on bacterial populations confirmed in general the inhouse findings that coliform counts decreased within 24 hours whereas heterotrophic plate counts increased over time. MSU is modifying a third draft of the final report and the FIU report is being peer reviewed. The University of Rhode Island completed the field testing for the project to develop an improved MF coliform medium. ------- APPROACH Solid Waste - DU D109 Page 47 ot jL. PE# fsfflA OUTPUT Quality Assurance A. C. ORD Contact Name Harry Kolde FTS No. 684-7325 Resources B. R/D 184.2 $(000) 195.2 PFT 0.1 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 18 Extramural Task: Develop and Maintain USEPA's Repository for Toxic and Hazardous Materials. Maintain the USEPA Repository for Toxic and Hazardous Materials to provide spiking/calibration solutions of organic compounds in support of monitoring under regulations of the Resource Conservation and Recovery Act (RCRA). Compounds of interest to RCRA are purchased or synthesized, purified, dissolved in appropriate solvents, and dispensed in 2 mL ampuls. The verity of pure compounds and concentration of the compound in the ampul are verified by referee laboratories. Upon verification, spiking/calibration solutions are advertised in the Quality Assurance Newsletter and distributed to USEPA, Regional, state, local, commercial, and RCRA contractor laboratories engaged in monitoring the environment. Accomplishments: 1. Of the 296 organic compounds listed in RCRA Appendix VIII, 272 compounds in neat form are in stock, of which 184 have been certified for purity, 132 analytes have been certified for distribution as calibration standards and 2 new standards are being tested for verity by referee laboratories. Purpose: Approach: 2. A total of 75,200 certified calibration standards were distributed to 1930 USEPA, Regional, state, local, and USEPA contract laboratories. This represents a 45% increase over FY85. 3. 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD)-native and calibration standards are certified for distribution. 4. Of the 247 compounds listed in the RCRA Appendix IX ground water list, 223 are stocked as neats in the Repository and 152 are available as calibration standards. Status: Annual Report of Repository Activities Completed (12/85) ------- Page 2 of Project No. 18 APPROACH Solid Waste - DU D109 Page 48 of 76 PE# B5U1A OUTPUT Quality Assurance A. C. 0RD Contact Name Terry Grady FTS No. B84-7325 Resources B. R/D $127 $(000) 141.6 PFT 0.2 0PFT PFTE 0PFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 18 Extramural Task: Conduct Verification Analyses on all performance evaluation (PE)/ quality control (QC) Samples. Usage of large numbers and types of QC, PE, and spiking/calibration samples in USEPA programs to assess the quality of monitoring data necessitates that true or reference values associated with the samples are in fact, valid. Otherwise poor decisions will result which could adversely impact the environment. Therefore, referee laboratories are used to establish the veracity of all samples. Referee laboratories are selected through the competitive procurement process upon the basis of performance evaluation and cost for the analytes of interest. These analytes include trace metals, nutrients, minerals, sodium and corrosivity, demand, trace organics in samples designed for gas chromatograph (GC) and GC/mass spectrometer (MS), polychlorinated biphenyls (PCBs) in oil, fish and sediment, and synthetic organic contaminants specified in the Organic Resources Conservation and Recovery Act (RCRA) Appendix VIII compounds. Accomplishments: Referee laboratories conducted: (1) 426 neat organic analyses to establish purity of materials in USEPA's Repository for Toxic and Hazardous Materials, (2) 3,668 analyses on QC and PE samples produced inhouse and on contract, (3) 402 analyses on spiking/ calibration solutions from USEPA's Repository for Toxic and Hazardous Materials, (4) No analyses on neat surrogates related to USEPA Methods 624 and 625, and (5) analyses on 18 spiking/ calibration solutions for surrogate compounds related to USEPA Methods 624 and 625. Purpose: Approach: Status: Annual Report of Referee Analytical Services Completed (12/85) ------- Page 3 of Project No. 18 Paqe 49 of 76 APPROACH PE# BSD1A Solid Waste - DU D109 Performance evaluations and waste characterization C. ORD Contact OUTPUT for Agency and contract laboratories. Name Harold Clements A. FTS No. 684-7325 B. $(000) 80.7 PFT 1.1 OPFT PFTE OPFTE Inhouse Task; Purpose: Approach: Accomplishments: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 18 Prepare Solid Waste Samples as Unknowns for Performance Evaluation (PE) Studies Evaluate the skills of Resource Conservation and Recovery Act (RCRA) contract laboratories. Develop a series of typical natural waste samples which are stable, homogeneous, and capable of analyses as routine samples. PE samples were prepared and distributed to RCRA contract laboratories for: 1. Interlaboratory Comparison Study V: Organic and inorganic type solid waste samples were sent to 20 RCRA laboratories in January 1986. Results of the Quality Assurance (QA) Branch and referee laboratories were returned to Office of Solid Waste (0SW). 2. Interlaboratory Comparison Study VI: Organic and inorganic samples were prepared and distributed to 50 USEPA, USEPA contractor, and other RCRA laboratories. The QA Branch and its referee laboratories analyzed the samples and provided statistical estimates to the OSW. The OSW developed acceptance limits for evaluating participating laboratories. 3. Interlaboratory Comparison Study VII - Diatomaceous earth and clay were used as a base to prepare a solid waste samples spiked with selected Appendix VIII compounds. The PE samples were sent in July 1986 to 50 laboratories for testing. The inorganic and the organic samples were analyzed by the QA Branch and Its referee laboratories and the results sent to OSW. 4. Design of new samples for the next study is in the pilot stage. Status: Reports: PE Samples for RCRA Contract Laboratories Completed (12/85) ------- Page 4 of Project No. 18 APPROACH Solid Waste - DU D109 Page 50 of 76 PE# USUI A OUTPUT Quality Assurance A. • C. ORD Contact Name Ed Berq FTS No. 684-7325 Resources B. R/D $64.9 $(000) 70.9 PFT 0.1 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 18 Extramural Task: Maintain USEPA's Quality Control (QC) Sample Program for Water-related Analytes. Purpose: QC samples are provided to USEPA, USEPA contractor, regional, state, and local laboratories as a check on the analyst's technique and analytical methodology. Such checks are necessary to monitor quality of data being generated in carrying out mandates of the Resource Recovery and Conservation Act (RCRA). Approach: Bionetics, Inc., the technical service contractor, provides personnel to develop, produce, and distribute QC samples. Development of new sample types requires: obtaining chemicals of the highest purity from best sources including the USEPA Repository for Toxic and Hazardous Materials, selecting the methodology for the compounds of interest, conducting retention time studies, and finally combining groups of organic compounds to minimize overlapping gas chromatog- raphy peaks and conducting 0, 45, and 90 day stability studies. Those compounds proven stable are produced at one concentration level in lots of 5,000. Random samples are withdrawn during production and sent to referee laboratories for verification. Upon verification, the new samples are advertised in the USEPA Quality Assurance Newsletter and distributed to requesters. Accomplishments: 1. A total of 285,167 QC samples were distributed to USEPA, USEPA contractor, state, and local laboratories. 2. A total of 181,000 ampuls were produced to replenish depleted inventories and included such QC series as trace metals, cyanide, polychlorinated biphenyls (PCBs) in oil and acetone, pesticides, and seven volatile organic series. 3. Of the 369 analytes listed in Appendix VIII, 119 are available for distribution. Status: Annual Report of QC Sample Program Completed (12/85) ------- Page 5 of Project No. 18 Sol id APPROACH Waste - DU D109 Page 51 of 76 PE# TES1A OUTPUT Continue NBS Traceability A. C. ORD Contact Name John Winter FTS No. 684-7325 Resources B. R/D $20K $(000) 20 PFT 0.0 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 18 Extramural Task: Establish Traceability of Quality Control (QC) and Performance Evaluation (PE) Samples to the National Bureau of Standards (NBS). Purpose: The QC and PE samples utilized throughout the United States and internationally in water/wastewater related monitoring programs must be of known quality since they are involved in many important decisions. As such, there is a stringent quality assurance program to assure the veracity of the QC and PE samples, the program for traceability to the NBS is established. Approach: An interagency agreement (IAG) was signed with NBS to develop a protocol for traceability of QC and PE samples, and then to implement the protocol for those analytes of interest to the Agency for which NBS has expert analytical capabilities. Accomplishments: NBS verified concentrations thereby establishing traceability for pesticides (lindane, endrine and methoxychlor), two herbicides (2,4-D and Silvex), and 14 volatile organic contaminants (trans and cis 1,2-dichloroethylene, dibromochloropropane, o-dichlorobenzene, ethylbenzene, chlorobenzene, sytrene, toluene, xylene, ethylene dibromide, chloroform, bromodichloromethane, dibromochloromethane and bromoform). Seven sludges which are to be used in an interlaboratory SW-846 method validation study are currently being analyzed for trace metals. Status: Annual Report on NBS Traceability Completed (12/85) ------- Page 6 of Project No. 18 Page 52 of /b APPROACH PE# BSD1A Solid Waste - DU D109 C. ORD Contact OUTPUT Externalization of QA Programs. Name John Winter A. FTS No. 684-7325 Resources B. R/D $ OK $(000) 0 PFT 0 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 18 Inhouse Task: Externalization of Quality Assurance (QA) Programs. Purpose: Recover costs of production, distribution, and administration of quality control (QC) and performance evaluation (PE) sample programs associated with the drinking water, industrial waste, and water quality program. Approach: Promulgate a cost recovery rule for the preparation and distribution of QC and PE samples, set up a mechanism for collecting such fees through the USEPA Financial Management Office, and begin the externalization process for these sample types. Accomplishments: An externalization task force was formed of USEPA personnel from the Comptroller's Office; Office of General Counsel; Office of Program Management; Office of Acid Deposition, Environmental Monitoring and Quality Assurance (OADEMQA); operating program offices; the regional offices; and the three EMSL laboratories to study and recommend the best option for externalization of QA support services. Concur- rently, EMSL-Cincinnati prepared a white paper on costs, for consideration by the Task Group. Discussions were also held between the Contracts Management Division and EMSL-Cincinnati to explore the best means to charge and collect user fees for these services and to expedite return of funds to EMSL-Cincinnati for maintenance of the QA program. Based on these deliberations and discussions, OADEMQA prepared a draft of a proposed rule: Proposed User Charges for Certain Quality Control and Performance Evaluation Samples Under the Clean Water Act and the Safe Drinking Water Act which was subsequently published in the Federal Register on September 16, 1986. Comments are due by October 31, 1986. Status: Report on the Externalization QA Program Completed (5/86) ------- Page 7 of Project No. 18 APPROACH Solid Waste - DU D109 OUTPUT Quality Assurance A. C. ORD Contact Name Ed B FTS No. Rpcnnrrp^ B. R/D $ OK $(000) 0 PFT 0 OPFT PFTE OPFTE Inhouse Task; Purpose: Approach: Accomplishments: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 18 Performance Evaluation (PE) Samples for the Ground Water Monitoring Program. Evaluate the performance of laboratories providing analyses of ground water samples collected at selected hazardous waste sites. A set of organic and inorganic PE samples are prepared by Bionetics, Inc., and sent to the field sample collection team at the hazardous waste stie. The PE samples are integrated into the samples collected at the site and then sent to laboratories under contract to USEPA. The analytical results scored were based upon past PE studies, interlaboratory method studies, analytical methods, and other sources. The PE samples for 15 sites were prepared and sent to two different groups of contract laboratories. These results were then used to help assess the quality of data being generated by the contract laboratory for each site by a panel consisting of personnel from EMSL-Las Vegas, EMSL-Cincinnati and the Office of Solid Waste (Headquarters), ICAIR Life Systems, and the regional offices. Status: Status Report on PE Samples for the Ground Water Monitoring Laboratories On Schedule (12/86) ------- APPROACH Solid Waste - DU D109 Page 54 of 76 PE# ES1J1A OUTPUT Interlaboratory Method Study A. C. ORD Contact Name Ray Wesselman FTS No. 684-7325 Resources B. R/D $325K $(000) 325 PFT 0 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 19 Extramural Task: Conduct interlaboratory method validation studies (IMVSs) to obtain precision and bias statements for USEPA Solid Waste (SW) 846 methodology. Purpose: In support of the Resource Conservation and Recovery Act (RCRA), IMVSs are conducted for USEPA analytical methdology to establish precision, bias, and other statistical estimates of performance. Such statistics are used to develop enforcement limits, establish quality control (QC) charts during routine analyses of pollutants, and provide confidence limits for QC samples. Approach: MVSs are conducted by a prime contractor involving 10 laboratories selected by USEPA. The selection is based upon laboratory experience with similar analyses, and performance on similar analytes. The prime contractor prepares three Youden pairs of samples as concentrates, each containing compounds specified in the method. The participating laboratories spike the concentrates into reagent water and solid waste matrices and analyze them according to the USEPA SW-846 methods. Analytical data are processed with the IMVS computer program which provides regression equations for recovery and precision and other statistics. Final reports are prepared for each USEPA method. The regression equations are used to develop performance criteria which are then incorporated into the method write-up. Accomplishments: A request for proposal (RFP) was developed and sent to perspective participants in the IMVS for SW-846 Method 8270, Base/Neutrals. Technically-acceptable laboratories received PE samples and 10 laboratories selected based on good performance. The IMVS should commence early in FY87. Status: Status Report: IMVS on SW-846 Method 8270 On Schedule (9/87) ------- Page 2 of Project No. 19 APPROACH Solid Waste - DU D109 Page 55 of 76 PE# ESUIA OUTPUT Interlaboratory Method Study A. C. ORD Contact Name Ray Wesselman FTS No. 684-7325 B. R/D $325K $(000) 325 PFT 0 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 19 Extramural Task: Conduct interlaboratory method validation studies (IMVSs) to obtain precision and bias statements for USEPA Solid Waste (SW) 846 methodology for Acrolein and Acrylonitrile. Purpose: In support of the Resource Conservation and Recovery Act (RCRA), IMVSs are conducted for USEPA analytical methdology for the purpose of established accuracy, precision, and other statistics. Such statistics are used to develop enforcement limits, establish quality control (QC) charts during routine analyses of pollutants, and provide confidence limits for QC samples. Approach: MVSs are conducted by a prime contractor using 10 laboratories selected by USEPA based upon their performance with similar analyses and performance on similar analytes. The study includes analyses of three Youden pairs of ampul concentrates containing the compounds specified in the analytical method. The participating laboratories spike the concentrates into reagent water and solid waste matrices and analyze them according to the USEPA SW-846 methods. Analytical data are processed with the USEPA IMVS computer program which provides regression equations for bias and precision and other statistics. Final reports are prepared for each USEPA method. Accomplishments: The IMVS for acrolein and acrylonitrile was temporarily delayed until research and development work can be completed on the analytical procedure. Status: Status Report: IMVS on SW-846 Method 8230 Acrolein and Acrylonitrile On Schedule (9/87) ------- Page 3 of Project No. 19 APPROACH Solid Waste - DU D109 Page 56 of 76 PE# BSD1A OUTPUT Interlaboratory Method Study A. C. ORD Contact Name Ed Berq FTS No. 684-7325 Resources B. R/D $0K $(000) 0 PFT 0 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 19 Extramural Task; Conduct interlaboratory method validation study (IMVS) to obtain precision and accuracy statements for USEPA Solid Waste (SW) 846 methodology for Trace Metals by Atomic Absorption (AA). Purpose: In support of the Resource Conservation and Recovery Act (RCRA), IMVSs are conducted for USEPA analytical methdology for the purpose of established accuracy, precision, and other statistics. Such statistics are used to develop enforcement limits, establish quality control (QC) charts during routine analyses of pollutants, and provide confidence limits for QC samples. Approach: MVSs are conducted by a prime contractor using 10 laboratories selected by USEPA based upon their performance with similar analyses and performance on similar analytes. The study includes analyses of three Youden pairs of ampul concentrates containing the compounds specified in the analytical method. The participating laboratories spike the concentrates into reagent water and solid waste matrices and analyze them according to the USEPA SW-846 methods. Analytical data are processed with the USEPA IMVS computer program which provides regression equations for bias and precision and other statistics. Final reports are prepared for each USEPA method. Accomplishments: A request for proposal (RFP) was developed and sent to prospective participants in the IMVS for SW-846 methods 3005, 3010, and 3050 - Trace Metals by atomic absorption (AA)-Flame. Technically acceptable laboratories received PE samples and 10 laboratories were selected from the good performers. The IMVS should commence early in FY87. Status: Status Report: IMVS on SW-846 Methods 3005, 3010, and 3050 - Trace Metals by AA-Flame On Schedule (9/87) ------- Solid Waste Research Corranittee Page 57 of 76 PE No. BSWT A. OUTPUT: Evaluated Analytical Monitoring Methods C. ORD Contact for Waste Characterization Name: J.J. Lichtenberq FTS No. 684-7306 B. RESOURCES: £1206.3 K FTE 7.0 FY 86 ANNUAL REPORT Project No. 20 Purpose and Approach The purpose of this project is to develop, evaluate, and validate extraction and analysis procedures for the identification and measurement of hazardous waste components including those not amenable to gas chromatographic tech- niques. Appropriate analytes listed in 40 CFR, Appendix VIII, Appendix IX, and the Michigan list will be studied to determine the applicability of gas chromatography (GC), GC-mass spectrometry (MS) and liquid chromatography (LC)-MS techniques to analysis of these compounds. Analytical methods published in SW-846 "Test Methods for Evaluating Solid Wastes - Physical/ Chemical Methods" will be evaluated. Progress and Accomplishments A "Report on Evaluation of Metals Dissolution for Chromium", deliverable Item No. 1696[A] was delivered to the Office of Solid Waste (OSW) on September 26, thus concluding this phase of the project to improve hexavalent chromium methodology. Evaluation of SW-846 Methods 8320 and 8330 - The project was initiated this quarter by Technology Applications, Incorporated (TAI), our in-house contractor. Retention times and chromatographic conditions have been established for revelant Appendix VIII analytes. Preliminary solubility and extraction efficiency studies have been performed. Several solvent solubility problems were identified. Testing and Evaluation of OSW Methods 8010/8015/8020 and Single Laboratory Validation of each Method - The draft final report has been received, reviewed, and returned to Battelle for extensive revision. Most analytes tested were considered to be within the scope of the method tested. However, the study identified a few analytes for each method that produced poor chromatography or purged very inefficiently. These are noted in the report. Testing and Evaluation of SW-846 Method 8240 - The reorientation of this effort toward capillary column chromatography has been underway. Testing both in-house and at Battelle has confirmed the scope of the method for water and solids. As a result, several additional analytes formerly assigned to solvent extraction methods are now being tested for inclusion in the broadened scope purge-trap-desorb (PTD) method. A status report in the form of comments on the Appendix IX proposal were submitted to OSW in September. ------- Page _2_ of Project No. 20 Page 58 of 76 Development of a Method for Formaldehyde to Replace SW-846 Methods 8410 and 8411 (Polarographic Procedures) for underground water and solid wastes - A draft final report on cartridge extractors and single laboratory validation of an high performance liquid chromatography (HPLC) method was submitted by Battelle in September. It has been reviewed and returned for revision. The cartridge extraction method showed promise but was subject to significant variations between suppliers of the extractors. Work on this project is continuing in an effort to resolve interference problems and reaction of formaldehyde precursors which tend to form formaldehyde during the analysis. Testing and Evaluation of SW-846 Method 8270 - The scope of 8270/3510 was established by determining which of the 127 compounds found to be within the scope of 8270 were extractable by the 3510 base-neutral/acid extraction protocol. These results reported to 0SW for its use within the Appendix IX comment period. Evaluation of Clean-up Procedures for Organics Included in the SW-846 Methods Manual - The contract intended to address this project was awarded to S-Cubed in the last week of September. A mid-October meeting was held at the contrac- tor site to finalize the workplan. Development of a Heated PTD Method for Intractable Volatile SW-846 Analytes - The Appendix VIII meeting participants (December 9-13, 1985) identified 13 intractable volatile analytes. Currently no method, other than direct aqueous injection, exists for their analyses. A work assignment has been issued to Battelle-Columbus Laboratories for them to investigate the possibility of developing a heated PTD method for these analytes. The chromatographic work has progressed well. The wide-bore polar columns (Carbowax-1ike) have demonstrated excellent separations and peaks. A problem exists with the instrument transfer lines. The polar materials such as acetone partition into condensed vapors, requiring all lines to be heated above 100"C. ------- Page 59 of 76 Solid Waste Research Committee PE No. BSD1A A. OUTPUT: Development of New Methods for Analysis C. ORD Contact of Solid Wastes Name: W. L. Budde FTS No. 684-7309 B. RESOURCES: $ 70.0 K FTE 0.0 FY 86 ANNUAL REPORT Project No. 21 Purpose and Approach The purpose of this project is to develop and evaluate liquid chromatography/ mass spectrometry (LC/MS) methods for nonvolatile non-gas chromatographable compounds on Appendix VIII of the Resource Conservation and Recovery Act (RCRA) regulations. Evaluation of a state-of-the-art thermospray interface for LC/MS will be done under a cooperative agreement with Cornell University. Progress and Accomplishments Work continued at Cornell University during the year. A LC/MS system was utilized to investigate methods for nonvolatile hazardous substances. Emphasis continued to be placed on methods for carbamate, amide, urea, and triazine pesticides that are not amenable to gas chromatography (GC) and for which no generic methods exist. These compounds appear on the Appendix VIII list of the RCRA regulations. A deliverable, Item 1678[A], "Report on Evaluation of Thermo- spray for MS/MS" is scheduled for delivery in December 1986. ------- APPROACH Solid Waste - DU D109 Page 60 of 76 PE# T55&1A OUTPUT Dioxin Method/QA A. C. ORD Contact Name Harry Kolde FTS No. "684-7325 Resources B. $(000) 100 PFT 0.0 OPFT PFTE OPFTE Extramural Task: Purpose: Approach: Accomplishments: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 22 Reference materials for chlorinated and brominated dibenzo-p-dioxins and dibenzo-furans at ppt level. Provide quality assurance support to dioxin monitoring committee. As an extramural effort, prepare or purchase, and purify, as necessary, dioxin and benzo-furan compounds. Prepare solutions of known concentrations. Verify qualitatively and quantitatively and distribute to DMP laboratories. Begin effort with the most toxic compounds, i.e., the isomers of 2,3,7,8 dioxin and benzofuran. If resources are available the brominated dioxin series and benzofurans will be purchased. The following chemicals were obtained in FY86: 50 mg each of tetra- bromodibenzo-p-dioxin (BDD), penta-BDD, hexa-BDD and octa-BDD, 50 mg of tetrachlorodibenzofuran (TCDF) and 5 mg of it as ^o^-labelled TCDF. Delivery of hepta-BDD is awaited. All funds allocated for this project through FY86 have been expended.. Status: Report - Purchase of Reference Materials for the Dioxin Monitoring Program Completed (12/85) ------- Solid Waste Research Committee Page 61 of 76 PE No. BSTHTT A. OUTPUT: Analytical Methods and Quality Assurance C. ORD Contact Guidance for Dioxin Monitoring Name: W. L. Budde FTS No. 684-7309 B. RESOURCES: $130.0 K FTE 0.0 FY 86 ANNUAL REPORT Project No. 23 Purpose and Approach The purpose of this extramural project is to develop and evaluate analytical procedures to identify and measure tetra-, penta-, hexa-, hepta-, and chlorinated octachlorodibenzo dioxins (CDDs) and chlorinated dibenzofurans (CDFs) in environmental samples. The project will be carried out under a contract with Battelle-Columbus laboratories. Progress and Accomplishments An internal report, titled "Automated Procedures for Mass Spectrometric Determination of Polychlorinated Dibenzo-p-dioxins and Polychlorinated Dibenzofurans by Isomer Class", was delivered to the program office in February, 1986. Under an interagency agreement with the Lawrence Livermore Laboratory of the Department of Energy, excellent progress was made in the effort to develop an immunochemical method for dioxins and furans. An enzyme linked immunosorbent assay (ELISA) was developed using the antibodies described in the last report. The assay proved to be highly reproducible and sensitive. A presentation on this work was made at a seminar in Cincinnati on August 7, 1986 and at the 6th International Symposium on Chlorinated Dioxins and Related Compounds, September 16, 1986 in Fukuoka, Japan. Another internal report on the "Development of Analytical Methods for Dioxins and Furans" is scheduled for delivery in December, 1986. ------- Page 2 of Project No. 23 Page 62 of 76 Solid Waste Research Committee PE No. BSD1A A. OUTPUT: Analytical Methods and Quality Assurance C. ORD Contact Guidance for Dioxin Monitoring Name: W. L. Budde FTS No. 684-7309 B. RESOURCES: $130.0 K PFTE 0.0 FY 86 ANNUAL REPORT Project No. 23 Purpose and Approach The purpose is to provide standard approaches for sampling and analysis of 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) and other chlorinated dibenzo-p-dioxins and chlorinated dibenzofurans (CDFs) in environmental samples and to provide quality assurance procedures which document the precision and accuracy. Emphasis will be placed on procedures to identify and measure tetra-, penta-, hexa-, hepta-, and octachlorodibenzo dioxins (CDDs) and CDFs. Existing procedures will be reviewed and evaluated and standard methods for sampling and measurement will be prepared. Accomplishments and Results to Date Full scan mass spectra were acquired for 20 CDD and CDF congeners. A computer data library was built and verified for correctness. Initial testing of an automated identification procedure was begun. Efforts are being made to acquire additional standards through an exchange with another agency that has an intensive systhesis program underway. Identification and Measurement of tetra-, penta-, hepta, and octachlorodi- benzodioxins and dibenzofurans in environmental samples - The work assignment was completed on schedule and a draft journal article titled "Automated Procedures for Mass Spectrometry Determination of Polychlorinated Dibenzo-p-dioxins and Polychlorinated Dibenzofurans by Isomer Class" was delivered. This document will be reviewed and modified for a scheduled FY 87 deliverable. Software to support this method through automated raw data interpretation and computations was also delivered. During FY 87 both the method and the software will be extensively tested, debugged, and documented. ------- Page 63 of 76 Superfund - Hazardous Emergency Response PE No. F6Y1A Committee A. OUTPUT: Monitoring Methods and QA Support for C. ORD Contact Situation Assessment Name: J.J. Lichtenberg FTS No. 664-7306 B. RESOURCES: % 0.0 K FTE 2.5 FY 86 ANNUAL REPORT Project No. 24 Purpose and Approach The purpose of this work is to provide guidance on sampling and analysis procedures, instrumentation and quality assurance that will allow decision makers to establish priorities between sites and provide scientific basis for decisions. The latest techniques and instrumentation will be applied to provide accurate information. An electronic data transfer system will be developed to collect and manage analytical data generated by the Superfund program. Progress and Accomplishments A report titled "The Need for Automated Data Handling in Environmental Monitoring" was delivered to the program office early in FY 86. In-house work was devoted to the support of the contract laboratory program (CLP) multilaboratory test of Method 680 for "Determination of Pesticides and PCBs in Water and Soil/Sediment by Gas Chromatography/Mass Spectrometry" which was revised after receiving comments from program offices, laboratory directors, and regional division directors. The method is supported by specialized software which automates the interpretation of the raw data and completes the calculations required for the polychlorinated biphenyl (PCB) level of chlorination approach. A document titled "Users' Guide for Software for Automated Identification and Measurement of Pesticides and Polychlorinated Biphenyls" and copies of the software prepared for this purpose, have been sent to many laboratories interested in field testing the method. Data from a six-laboratory collaborative study of the method were extensively analyzed and an oral report on the study was made at the CLP program meeting in August. Further information on the method and study was presented at the CLP October 1986 meeting. ------- APPROACH Superfund - DU Y105 Page 64 of 76 PE# IHT71A OUTPUT Monitoring and QA Support for Situation Assessment. A. C. ORD Contact Name Ed Berq FTS No. 684-7325 Resources B. R/D $(000) 56 PFT 0.2 OPFT PFTE OPFTE FY84 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 25 Extramural Task: Performance Evaluation (PE) of Superfund Contractors. Purpose: Quality assurance (QA) support is needed for USEPA and USEPA contractor laboratories for Superfund. Some measure of performance is needed to monitor the quality of data generated by Comprehensive Environmental Response Compensation and Liability Act (CERCLA) laboratories. Approach: Natural wastewater samples are prepared, verified as to concen- tration, and distributed in quarterly evaluations of Superfund contract laboratories, in cooperation with EMSL-Las Vegas. Accomplishments: Full-volume natural wastewater samples spiked with approximately 20 compounds were prepared and shipped to approximately 60 Superfund contract laboratories, and to USEPA Regional laboratories once each quarter. Concentration levels were designed for gas chromatograph/ mass spectrometer (GC/MS) capillary analyses and included volatiles and semi-volatiles. Verification analyses were conducted on the full-volume samples and data submitted to EMSL-Las Vegas. In the first, second, and third quarters, samples were sent to Regions 1, 6 and 7 for distribution to Contract Laboratory Program (CLP) laboratories. During the fourth quarter, the samples were sent directly to prospective CLP laboratories as preaward PE samples. Status: Annual Report on PE of Superfund Contractors Completed (12/85) ------- Page 2 of Project No. 25 APPROACH Superfund - DU Y105 Page PE# 65 of 76 ESV1A OUTPUT Monitoring and QA Support for Situation Assessment. A. C. ORD Contact Name Ed Berg FTS No. 684- -7325 Resources B. $(000) 126 PFT 0.1 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 25 Extramural Task: Maintain USEPA's Quality Control (QC) Sample Program for Water-related Analytes. QC samples are provided to USEPA, regional, state, and USEPA contractors as a check on the analyst technique and analytical methodology. Such checks are necessary to monitor the quality of data being generated in carrying out mandates of the Resource Conservation and Recovery Act (RCRA). Bionetics, Inc., the technical service contractor, provides personnel to develop, produce, and distribute QC samples. Development of new sample types requires obtaining chemicals of the highest purity such as those from the USEPA Repository for Toxic and Hazardous Materials, selecting the methodology for the compounds of interest, conducting retention time studies, and finally combining groups of organic compounds to minimize overlapping gas chromatography peaks and conducting 0, 45-, and 90-day stability studies. Those compounds proven stable are produced at one concentration level in lots of 5,000. Random samples are withdrawn during production and sent to USEPA referee laboratories for verification analyses. Upon verification, the new sample is advertised in the USEPA Quality Assurance (QA) Newsletter and distributed to requesters. Accomplishments: 1. A total of 285,167 QC samples were distributed to USEPA, regional, state, local, and USEPA contractor laboratories. 2. A total of 181,000 ampuls were produced to replenish depleted inventories and included such QC series as trace metals, cyanide, polychlorinated biphenyls (PCBs) in oil, PCBs in acetone, pesticides, and seven volatile organic series. 5. Of the 618 analytes listed in Appendix A, 135 are available for distribution. Purpose: Approach: Status: Annual Report of QC Sample Program Completed (12/85) ------- Page 3 of Project No. 25 APPROACH Superfund - DU Y105 Page 66 of 76 PE# ESYlA OUTPUT Monitoring and QA Support for Situation Assessment. A. C. ORD Contact Name Harry Kolde FTS No. 684-7325 Resources B. R/O $(000) 106 PFT 0.1 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 25 Extramural Task: Develop and maintain USEPA's Repository for Toxic and Hazardous Materials. Purpose: Maintain the USEPA Repository for Toxic and Hazardous Materials to provide spiking/calibration solutions of organic compounds in support of monitoring under Comprehensive Environmental Response Compensation and Liability Act (CERCLA) regulations. Approach: Compounds of interest to Superfund (SF) are purchased or synthesized, purified, dissolved in the appropriate solvent, and dispensed in 2 mL ampuls. The purity of pure compounds and concentrations in the ampuls are verified by referee laboratories. Upon verification, spiking/calibration solutions are announced in the Quality Assurance Newsletter and distributed to USEPA, SF contractor, state, and local laboratories engaged in SF monitoring the environment. Accomplishments: Approximately 608 compounds are specified in the Appendix A List. The Repository contains 480 of these as neat materials in stock; 228 of the neat materials have been certified for purity and 156 certified analytes available for distribution; and nine new chemicals are currently being tested by referee laboratories. Status: Annual Report of Repository Activities Completed (12/85) ------- Page 4 of Project No. 25 APPROACH Superfund - DU Y105 Page 67 of 76 PE# EG71A C. ORD Contact OUTPUT Monitoring and QA Support for Situation Assessment Name John Winter A. FTS No. 684-7325 B. R/D $ OK $(000) 0 PFT 0 OPFT PFTE OPFTE Inhouse Task: Purpose: Approach: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 25 Externalization of Quality Assurance (QA) Programs. Recover costs of production, distribution, and administration of quality control (QC) and performance evaluation (PE) sample programs associated with the drinking water, industrial waste, and water quality program. Promulgate a cost recovery rule for the preparation and distribution of QC and PE samples, set up a mechanism for collecting such fees through the USEPA Financial Management Office, and begin the externalization process for these sample types. Accomplishments: An externalization task force was formed of USEPA personnel from the Comptroller's Office; Office of General Counsel; Office of Program Management; Office of Acid Deposition, Environmental Monitoring and Quality Assurance (OADEMQA); operating program offices; the regional offices; and the three EMSL laboratories to study and recommend the best option for externalization of QA support services. Concur- rently, EMSL-Cincinnati prepared a white paper on costs, for consideration by the Task Group. Discussions were also held between the Contracts Management Division and EMSL-Cincinnati to explore the best means to charge and collect user fees for these services and to expedite return of funds to EMSL-Cincinnati for maintenance of the QA program. Based on these deliberations and discussions, OADEMQA prepared a draft of a proposed rule: Proposed User Charges for Certain Quality Control and Performance Evaluation Samples Under the Clean Water Act and the Safe Drinking Water Act which was subsequently published in the Federal Register on September 16, 1986. Comments are due by October 31, 1986. Status: Report on the Externalization OA Proqram Completed (5/86) ------- Page 5 of Project No. 25 APPROACH Superfund - DU Y105 Page 68 PE# rGY of 76 1A OUTPUT Quality Assurance A. C. ORD Contact Name Ed Bi FTS No. Resources B. R/D $ OK $(000) PFT OPFT PFTE OPFTE Inhouse Task: Purpose: Approach: Accomplishments: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 25 Performance Evaluation (PE) Samples for the Ground Water Monitoring Program. Evaluate the performance of laboratories providing analyses of ground water samples collected at selected hazardous waste sites. A set of organic and inorganic PE samples are prepared by Bionetics, Inc. and sent to the field sample collection team at the hazardous waste site. The PE samples are integrated into the samples collected at the site and then sent to laboratories under contract to USEPA. The analytical results scored based upon past PE studies, interlaboratory method studies, and other sources. Separate PE samples were prepared for 15 sites and sent to two groups of contract laboratories. The results were then used to help assess the quality of data being generated by the contract laboratory for each site. A panel of personnel from EMSL-Las Vegas, EMSL-Cincinnati and the Office of Solid Waste (Headquarters), ICAIR Life Systems, and the regional offices reviewed the results of the quality assurance work and agreed in a concensus evaluation for each site, through telephone conference calls. Status: Status Report on PE Samples for the Ground Water Monitoring Laboratories On Schedule (12/86) ------- Paqe 69 of 76 APPROACH PE# E6Y1A Superfund - DU Y105 C. ORD Contact OUTPUT Provide Technical Support to Enforcement Program Name Harold Clements A. FTS No. 684-7325 PpcnurrPQ B. $(000) 7 PFT 0.1 OPFT PFTE OPFTE Inhouse Task: Purpose: Approach: Accomplishments: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 26 Conduct Performance Evaluation Studies for Remedial Programs Evaluate performance of Hyde Park litigant laboratories in the Comprehensive Environmental Response Compensation and Liability Act (CERCLA) Program. Develop a series of samples which are stable and homogeneous and capable for use as unknown samples to conduct studies and evaluate results. The Quality Assurance (QA) Branch prepared and distributed samples to Hooker Chemical Company, Niagara Falls, New York in support of the Hyde Park agreement. Twenty-one target compounds were spiked into an organic solvent for gas chromatograph/mass spectrometer (GC/MS) analyses. Series VII and Series VIII were sent December 1985 and July 1986, respectively, to Hooker Chemical Company for analyses. The data were evaluated on return to the QA Branch and reported to the USEPA Hyde Park Litigation Program Coordinator in Region 2. Laboratory performance in these two studies was acceptable. The next study sample will be sent in December 1986. Status: Report of Technical Support to Region 2, Evaluation of Performance in Enforcement Action Completed (12/85) ------- 1 1 APPROACH I Manage Agency Mandatory Quality Assurance Program - DU Page 70 or 76 1 PE# 1 H109 1 I Technical Information and Management Support to 1 A. OUTPUT: Quality Assurance Management Staff (QAMS). I Communication between QAMS and EMSL-Cincinnati as 1 well as between QAMS and the Regional, Headquarters 1 and National Laboratory Quality Assurance Officers. C. UKD Contact 1 NAME: Daniel F. Bender I FTS No. 684-7301 I 1 1 1 RESOURCES: 1 B. $(000) 49.8 PFT 0.9 OPFT PFTE 1 OPFTE t 1 1 ANNUAL REPORT - FY86 PROJECT NUMBER 27 Purpose and Approach This project is an on-going function involving the supplying of technical and policy information and technical services such as document review, committee and work group membership, document and report preparation, and the coordination of the input into these activities of regional, headquarters, and national laboratory Quality Assurance Officers (QAOs). Accomplishments and Results to Date 1. Routinely-Used Measurement Method (RUMM) Work Group (WG): The RUMM compendium document was prepared for review by U.S. Environmental Protection Agency (USEPA) and state users. EMSL-Cincinnati's review was obtained. The contractor, Re- search Triangle Institute, the WG Chairman, and myself, reviewed the final changes with each individual EMSL-Cincinnati reviewer. EMSL-Cincinnati concurrence as to technical accuracy was obtained. After a teleconference with the Environmental Services Division (ESD) Directors, the compendium was reviewed by USEPA users and some state laboratories; a summary of comments was prepared. Several teleconfer- ences concerning the next phase of the RUMM project were held. USEPA Project Summaries for all of the EMSL-Cincinnati Method Validation Studies were gathered and transmitted to the WG Chairman for use in the next phase. 2. Audits: Prepared the "Follow-up Audit" section for the Office of Research and Development (ORD) Management Systems Audit (MSA) Protocol. 3. QAO Meetings: The annual FY 86 Fall QAO meeting was attended. The annual ORD QAO meeting was hosted by EMSL-Cincinnati. A newly organized series of bimonthly Regional QAO conference call meetings was initiated. The quarterly Andrew W. Breidenbach Environmental Research Center QAO meetings were held and the minutes were reported to Quality Assurance Management Staff (QAMS). The planning for the FY 87 Fall QAO meeting was initiated. 4. QA Document Preparation and Review: Assisted in the preparation of the EMSL- Cinclnnati Quality Assurance Program Plan (QAPP) (Parts 1 and 3) through several revisions. Reviewed the Office of Acid Deposition, Environmental Monitoring, and Quality Assurance (OADEMQA) QAPP through several revisions. Reviewed the Quality Assurance/Quality Control (QA/QC) Estuary Methods Manual for the Office of Marine and Estuary Protection. Prepared the 304(h) statement for residual chlorine. Reviewed the Quality Assurance Project Plan (QAPjP) for Underground Injection Control in Region 9. ------- Page 2 of Project No. 27 Page 71 of 5. Other Assignments: Participated in a National Association of Science Program Review of EMSL-Cincinnati QA activities. Reviewed an International Union of Pure and Applied Chemistry (IUPAC) document on sampling nomenclature. Worked on Standard Methods, 17th Edition Joint Task Groups (JTGs) on Residual Chlorine, Chlorine Dioxide, and Ozone. Participated, as a lecturer, in a laboratory short course at the University of Florida Training Research and Education for Environmental Occupations (TREEO) Center sponsored by the Florida Society of Environmental Analysts. Successfully completed the Chemical Laboratory Drinking Water Certification Course and the Contract Officer 40-Hour Certification course. Status: 1. RUMM WG: Method 624 is being prepared by the contractor for inclusion in RUMM. The Sampling Subgroup is preparing a strawman project summary outline based on a number of Standard Operating Procedures and sampling manuals obtained from Superfund, EMSL-Cincinnati, Region 4, and the Office of Solid Waste. 2. Audit: Several audits are being finalized; more active participation in future audits by the EMSL-Cincinnati Liaison is planned. 3. QAO Meeting: Participation in the Fall FY 87 national QAO meeting is planned. Input to the planned ORD QAO meeting and the Regional QAO meeting will be forthcoming. 4. QA Document Preparation and Review: EMSL-Cincinnati Liaison participation in a variety of QA and method development activities is expected. 5. Other Assignments: Participation in the Standard Methods JTGs will continue. Participation in two other JTGs was recommended by the EMSL-Cincinnati Director at the last Joint Editorial Board Meeting: Reagent Water and Safety. Partici- pation in the laboratory short course at the TREEO Center is anticipated. ------- Acid Deposition Research Program Office Page 72 of 76 PE No. CVNTTT A. OUTPUT: Wet Deposition Monitoring Methods C. ORD Contact Name: J.J. Lichtenberq FTS No. 684-7306 B. RESOURCES: $100.0 K FTE 0.0 FY 86 ANNUAL REPORT Project No. 28 Purpose and Approach The purpose is to provide improved methods for collection and analysis of Wet Precipitation Samples. The approach will be to develop and evaluate analyti- cal methods for inorganic ions and other parameters in atmospheric deposition samples under a cooperative agreement with the State of Illinois. Progress and Accomplishments A methods manual which includes methods for pH, Ca, Mg, K, Na, NH3, CI, NO3, PO4, SO4, F, and specific conductance has been published and a report on "Standard Methods for Collection and Analysis of Precipitation" was delivered to the program office in April 1986. A new cooperative agreement was awarded to the Illinois State Water Survey to evaluate methods for reactive aluminum. The project is scheduled to begin early in FY 87. Development and Evaluation of Methods for the Analysis of Ions in Atmospheric Deposition—A draft method, "Dissolved Aluminum, Cadmium, Copper, Iron, Lead, Manganese and Zinc in Wet Deposition by Graphite Furnace Atomic Absorption Spectrophotometry", has been received from the contractor. This draft method was reviewed and returned to the authors for revision. ------- APPROACH Chemical Assessment - DU L104 ^ge 73 of 2£L PE# CRL1A OUTPUT Quality Assurance for Toxic Substances A. C. ORD Contact Name John Winter FTS No. 684-7325 Resources B. R/D $20K $(000) 20 PFT 0 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 29 Extramural Task: Establish Traceability of Quality Control (QC) and Performance Evaluation (PE) Samples to the National Bureau of Standards (NBS). Purpose: The QC and PE samples utilized throughout the United States and internationally in water related monitoring programs must be of the high quality since they are involved in important decisions. As part of a stringent quality assurance program to assure the veracity of representative QC and PE samples, traceability to the NBS is established. Approach: An interagency agreement (IAG) was signed with NBS to develop a protocol for traceability of QC and PE analytes, and then to implement the protocol for top priority samples of interest to the Agency and those for which NBS has expert analytical capabilities. Accomplishments: NBS verified, thereby establishing traceability for the pesticides lindane, endrin and methoxychlor, two herbicides (2,4-D and Silvex), and 14 volatile organic contaminants (trans and cis 1,2-dichloro- ethylene, dibromochloropropane, o-dichlorobenzene, ethylbenzene, chlorobenzene, sytrene, toluene, xylene, ethylene dibromide, chloroform, bromodi- chloromethane, dibromochloromethane and bromoform). Seven sludges which are to be used in an interlabora- tory method validation study are currently being analyzed. Status: Annual Report on Traceability to NBS Completed (12/85) ------- Page 2 of Project No. 29 " Page 74 of 76 APPROACH PE# "CRU1A Chemical Assessment - DU L104 C. ORD Contact OUTPUT Quality Assurance for Toxic Substances Name Harry Kolde A. FTS No. 684-7325 Resources B. R/D $60.4 $(000) 60.4 PFT 0 OPFT PFTE OPFTE Extramural Task: Purpose: Approach: Accomplishments: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 29 Conduct Verification Analyses on performance evaluation/quality control (PE/QC) Samples. Usage of QC, PE, and spiking/calibration samples in the Toxics program to assess the quality of monitoring data necessitates that true or reference values associated with the samples are in fact, valid. Otherwise poor decisions could result which would adversely impact the environment. Therefore, referee laboratories are used to establish the veracity of samples. Referee laboratories are selected through the competitive procurement process upon the basis of performance evaluation and cost for the analytes of interest. These analytes include trace metals, polychlorinated biphenyls (PCBs) in oil, synthetic organic contaminants specified in Toxics regulations, and for other analytes regulated by the Agency. Referee laboratories conducted 74 analyses to confirm the veracity of PCB calibration standards. Status: Annual Report on Referee Analytical Services Completed (12/85) ------- Page 3 of Project No. 29 Page 75 of 76 APPROACH PE# URTlA Chemical Assessment - DU L104 C. ORD Contact OUTPUT Quality Assurance for Toxic Substances Name Ray Wesselman A . FTS No. 684-7325 Resources B. R/D $35 $(000) 35 PFT 0 OPFT PFTE OPFTE FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 29 Extramural Task: Prepare, Analyze, and Distribute Quality Control (QC) Samples. Purpose: QC Samples are provided to USEPA, USEPA contractor, state, and local laboratories as a check on the analyst's technique and analytical methodology. Such checks monitor the quality of data being generated by laboratories conducting analyses under the Toxic Substances Control Act (TSCA). Approach: Bionetics, Inc., the technical service contractor, develops, produces, and distributes QC samples. Development of new sample types requires obtaining chemicals of the highest purity from the best sources including the USEPA Repository for Toxic and Hazardous Materials, selecting the methodology for the compounds of interest to TSCA, conducting retention time studies, and combining groups of organic compounds to minimize overlapping gas chromatography peaks and conducting 0, 45-, and 90-day stability studies. Those compounds proved stable are produced at one concentration level in lots of 5,000. Random samples are withdrawn during production and sent to USEPA referee laboratories for verification analyses. Upon verification, the new sample is advertised in the USEPA Quality Assurance Newsletter and distributed to requesters. Accomplishments: • A total of 285,167 QC samples for all analytes were distributed to USEPA, state, local, and commercial laboratories engaged in water/wastewater monitoring. Produced the following sample series to replace depleted stocks: polychlorinated biphenyls (PCBs) 1254, 1248, 1260, 1016, and 1242 in acetone and in oils. A total of 181,000 ampuls were produced to replenish depleted inventories and included such QC series as trace metals, cyanide, PCBs in oil and acetone, pesticides, and seven volatile organic series. Participated in interlaboratory method study for PCBs monstration program for PCB distruction. The set consisted of PCB congeners (mono, di, tri, and tetra biphenyls) and Aroclors 1242, 1254, and 1260. Fifty sets of each were supplied to the Office of Toxic Substances (OTS). Status: Annual Report on QC Sample Program Completed (12/85) ------- Page 4 of Project No. 29 Page 76 of 76 APPROACH PE# flRTlA Chemical Assessment - DU L104 C. ORD Contact OUTPUT Quality Assurance for Toxic Substances Name Harry Kolde A. FTS No. 664-7325 Resources B. R/D $31.2 $(000) 31.2 PFT 0 OPFT PFTE OPFTE Extramural Task: Purpose: Approach: FY86 ANNUAL REPORT Quality Assurance Branch, EMSL-Cincinnati Project No.: 29 Develop and maintain USEPA's Repository for Toxic and Hazardous Materials. The USEPA Repository for Toxic and Hazardous Materials provides spiking/calibration solutions of organic compounds in support of regulations under the Toxic Substances Control Act (TSCA). Compounds of interest to the Office of Toxic Substances (OTS) are purchased or synthesized, purified, dissolved in the appropriate solvent, and finally dispensed in 1.5 mL ampuls. The verity of pure compounds and concentration of the compound in the ampul are verified by referee laboratories. Upon verification, spiking/calibration solutions are advertised in the Quality Assurance Newsletter and distributed to USEPA, USEPA contractor, state, and local laboratories engaged in monitoring the environment. Accomplishments: 1. 2. 3. A total of 75,200 certified calibration standards were distributed to 1930 USEPA, USEPA contractor, state, and local laboratories. This represents a 45% increase over FY85. Twenty different individual polychlorinated biphenyl (PCB) standards in methanol or isooctane solutions are now available. Sixty-five of the special PCB calibration standards containing the mono-, tetra-, octa-, and deca-chlorobiphenyl isomers were distributed to OTS contractors. Status: Annual Report on Repository Completed (12/85) ------- |